Method for producing magnetic microparticles, magnetic microparticles obtained therefrom, magnetic fluid, and method for producing magnetic product

ABSTRACT

It is an object to provide a method for producing magnetic microparticles, which produces monodispersed magnetic microparticles, causes no clogging with a product due to self-dischargeability, requires no great pressure, and is excellent in productivity. In the method for producing magnetic microparticles, at least two fluids are used, and at least one kind of the fluids is a fluid containing at least one kind of magnetic raw material, and at least one kind of the fluids other than the above fluid is a fluid containing at least one kind of a magnetic microparticles-separating agent, and the respective fluids join together in a thin film fluid formed between two processing surfaces arranged to be opposite to each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, whereby magnetic microparticles are separated in the thin film fluid to obtain the magnetic microparticles.

TECHNICAL FIELD

The present invention relates to a method for producing magneticmicroparticles and the like.

BACKGROUND ART

-   Patent Document 1: JP-A S61-36907-   Patent Document 2: JP-A 2005-123454-   Patent Document 3: JP-A 2005-48213-   Patent Document 4: JP-A 2005-97055-   Patent Document 5: JP-A 2007-165782

Some metals and metal compounds such as metal oxides, metal nitrides ormetal sulfides have so-called magnetic property such as being attractedor repulsed to a magnet. Those having such property are referred to asmagnetic bodies or magnetic substances. Microparticles of the magneticbody, that is, magnetic microparticles are utilized in a high densityrecording medium or magnetooptical recording medium used for such ascomputers, a magnetic tape, a electromagnetic wave-shielding material, atoner for electrophotograph and the like due to their magneticproperties. Further, a water purification agent such as an aggregatingagent comprising a magnet-binding polymer has been developed and a drugdelivery system using a magnetic imparting agent has also been developedin pharmaceutical industries.

Magnetic fluids are those in which the magnetic microparticles describedabove are dispersed in a medium such as oils or water in a colloidalstate. At the beginning of the 1960's, in NASA's space program, magneticfluids were developed for utilizing as the magnetic transporting controlof liquid fuels for rockets under weightless conditions in space, or asthe liquid encapsulation materials for space suits. Such magnetic fluidsare used at many sites such as an angle sensor, an inclination sensor, ashaft seal and a vibration damper, and a research for improving theproperty of the magnetic fluids has been promoted. For example, in aresearch for enlarging the saturation magnetization of the magneticfluids, there has been disclosed a technique relating to magnetic fluidscomprised of cobalt metal microparticles, surfactants and carbonaceouscatalysts (Patent Document 1).

In order to utilize the property of the magnetic microparticles, it isvery important to allow the magnetic microparticles to be monodispersedfor maintaining a coercive force while having a high coercive force,that is, to prepare magnetic microparticles having a uniform size, andthere is also the need for controlling the crystallinity and crystalform thereof.

The production methods include a method for obtaining magnetic fluidscontaining metal microparticles having an average particle size of 7 nmto 12 nm in high concentration by adding metal carbonyl to a hydrocarbonmedium in which a surfactant is dissolved and heating the mixture to bethermally decomposed as described in Patent Document 1, a method forcontrolling the particle size of metal microparticles to be prepared bythe reflux temperature of an organometallic compound solution dispersedin a solution when metallic magnetic fluids are produced in a solutionin the presence of a surfactant as described in Patent Document 2, and amethod for irradiating a dispersion slurry comprising amorphousparticles having a particle size of 0.5 nm to 100 nm whose surface isbound to organic coordination molecules with laser to heat the amorphousparticles, followed by crystallization (Patent Document 3). Further, amethod for producing composite oxide microparticles comprising thecalcining step of mixing and calcining two kinds of metallic oxidemicroparticles, at least one of which is a ferromagnetic oxide, in avapor medium at high temperature to prepare composite oxidemicroparticles in which both microparticles are melt and joined, and therapid cooling step of subjecting the vapor medium passed through thecalcining step to a magnetic field to isolate the composite oxidemicroparticles from the vapor medium and simultaneously to introduce thecomposite oxide microparticles into the cooling system, followed bypreparation of amorphous composite oxide microparticles by rapid cooling(Patent Document 4), and a method for preparing magnetic particles orprecursors of magnetic particles by introducing a raw material gas flowcontaining a metal constituting a magnetic body and a reactant gas flowcovering the raw material gas flow into a reaction space in ahigh-temperature atmosphere, forming microparticles through heatreaction at the periphery of the raw material gas flow andsimultaneously cooling the microparticles with the reactant gas flow(Patent Document 5).

However, the production method in which two or more kinds of organicsolvents are necessarily used in a large amount as described in PatentDocument 2, or the production method in which magnetic microparticlesafter reaction are subjected to specific post treatment or process asdescribed in Patent Document 3 highly possibly allows the steps to becomplicated, and the time requiring for the production to be prolonged.When the method such as Patent Document 4 or 5 is used, there is aproblem such that an apparatus having an expensive and complicatedmechanism is necessarily used and therefore, it is concerned that thevalue of a product is naturally high. All the problems lie in the factthat a problem of aggregation and control of crystallinity, which areeasily caused upon obtaining nano size magnetic microparticles, remainunsolved. That is, in the liquid phase reaction capable of easilyproducing magnetic microparticles, all the problems lie in the fact thathomogenization of particle size and unification of a reaction productcan not be effectively and efficiently carried out due to temperaturenonuniformity and stirring nonuniformity in a reactor.

In light of this situation, it is an object of the present invention toprovide a method for producing magnetic microparticles, the magneticparticles are obtained by allowing a magnetic raw material to react witha magnetic microparticles-separating agent in a thin film fluid formedbetween two processing surfaces arranged to be opposite to each other soas to be able to approach to and separate from each other, at least oneof which rotates relative to the other, wherein the temperature in thethin film fluid is highly uniform and the stirring in a reactor is alsohighly uniform so that monodispersed magnetic microparticles can beprepared depending on its purpose, and wherein clogging with a productdoes not occur due to self-dischargeability, great pressure is notnecessary, and productivity is high, magnetic microparticles obtainedtherefrom, and a magnetic fluid containing the same.

DISCLOSURE OF INVENTION

An aspect of the invention according to claim 1 in the presentapplication is a method for producing magnetic microparticles, whereinat least two fluids are used, wherein at least one kind of the fluids isa fluid containing at least one kind of a magnetic raw material, and atleast one kind of fluid other than said fluids is a fluid containing atleast one kind of a magnetic microparticles-separating agent, and therespective fluids join together in a thin film fluid formed between twoprocessing surfaces arranged opposite to each other so as to be able toapproach to and separate from each other, at least one of which rotatesrelative to the other, whereby magnetic microparticles are separated inthe thin film fluid to obtain the magnetic microparticles.

An aspect of the invention according to claim 2 in the presentapplication is the method for producing magnetic microparticlesaccording to claim 1, wherein at least one kind of the fluids contains adispersant.

An aspect of the invention according to claim 3 in the presentapplication is a method for producing magnetic microparticles, whereinat least two fluids are used, wherein at least one kind of the fluids isa reverse micellar solution obtained by adding a dispersant and at leastone kind of aqueous magnetic raw material solution to an organicsolvent, and at least one kind of fluid other than said fluids is areverse micellar solution containing at least one kind of a magneticmicroparticles-separating agent, and the respective fluids join togetherin a thin film fluid formed between two processing surfaces arrangedopposite to each other so as to be able to approach to and separate fromeach other, at least one of which rotates relative to the other, wherebymagnetic microparticles are separated in the thin film fluid to obtainthe magnetic microparticles.

An aspect of the invention according to claim 4 in the presentapplication is the method for producing magnetic microparticlesaccording to any one of claims 1 to 3, wherein the magneticmicroparticles contains at least one kind selected from nickel, cobalt,iridium, iron, platinum, gold, silver, manganese, chromium, palladium,yttrium, and lanthanides (neodymium, samarium, gadolinium and terbium).

An aspect of the invention according to claim 5 in the presentapplication is the method for producing magnetic microparticlesaccording to any one of claims 1 to 4, wherein the magneticmicroparticles contains at least one kind selected from copper, zinc,magnesium, rhenium, bismuth and silicon.

An aspect of the invention according to claim 6 in the presentapplication is the method for producing magnetic microparticlesaccording to any one of claims 1 to 5, wherein heat (warmth) is addedbetween the processing surfaces; ultraviolet ray (UV) is irradiatedbetween the processing surfaces; or ultrasonic energy is suppliedbetween the processing surfaces.

An aspect of the invention according to claim 7 in the presentapplication is the method for producing magnetic microparticlesaccording to any one of claims 1 to 6, wherein the separation reactionis conducted in a reactor capable of securing a depressurized or vacuumstate, at least to form a depressurized or vacuum state of the secondaryside at which the fluid after processing is discharged thereby beingcapable of removing a solvent in the fluid or a gas generated during theseparation reaction or a gas contained in the fluid.

An aspect of the invention according to claim 8 in the presentapplication is the method for producing magnetic microparticlesaccording to any one of claims 1 to 7, wherein the magneticmicroparticles have a volume-average particle size of 0.5 nm to 1000 nm.

An aspect of the invention according to claim 9 in the presentapplication is the method for producing magnetic microparticlesaccording to any one of claims 1 to 8, wherein the production methodincludes a fluid pressure imparting mechanism that imparts predeterminedpressure to a fluid to be processed, at least two processing members ofa first processing member and a second processing member capable ofrelatively approaching to and separating from the first processingmember, and a rotation drive mechanism that rotates the first processingmember and the second processing member relative to each other, whereineach of the processing members is provided with at least two processingsurfaces of a first processing surface and a second processing surfacedisposed in a position they are faced with each other; each of theprocessing surfaces constitutes part of a sealed flow path through whichthe fluid under the predetermined pressure is passed; two or more fluidsto be processed, at least one of which contains a reactant, areuniformly mixed and positively reacted between the processing surfaces;of the first and second processing members, at least the secondprocessing member is provided with a pressure-receiving surface, and atleast part of the pressure-receiving surface is comprised of the secondprocessing surface, the pressure-receiving surface receives pressureapplied to the fluid by the fluid pressure imparting mechanism therebygenerating a force to move in the direction of separating the secondprocessing surface from the first processing surface; and the fluidunder the predetermined pressure is passed between the first and secondprocessing surfaces being capable of approaching to and separating fromeach other and rotating relative to each other, whereby the processedfluid forms a fluid film of predetermined thickness while passingbetween both the processing surfaces, and the production method furtherincludes another introduction path independent of the flow path throughwhich the fluid to be processed under the predetermined pressure ispassed, and at least one opening leading to the separate introductionpath and being arranged in at least either the first processing surfaceor the second processing surface, wherein at least one processed fluidsent from the introduction path is introduced into between theprocessing surfaces, whereby the reactant contained in at least any oneof the aforementioned processed fluids, and a fluid other than saidprocessed fluid enable a state of desired reaction by mixing underuniform stirring in the fluid film.

An aspect of the invention according to claim 10 in the presentapplication is the method for producing magnetic microparticlesaccording to any one of claims 1 to 9, wherein the obtained magneticmicroparticles are excellent in re-dispersibility.

An aspect of the invention according to claim 11 in the presentapplication is magnetic microparticles produced by the production methodaccording to any one of claims 1 to 10.

An aspect of the invention according to claim 12 in the presentapplication is a magnetic fluid comprising the magnetic microparticlesproduced by the production method according to any one of claims 1 to10.

An aspect of the invention according to claim 13 in the presentapplication is a method for producing a magnetic product comprising atleast the magnetic microparticles produced by the production methodaccording to any one of claims 1 to 10.

The present invention relates to a method of producing magneticmicroparticles obtained by preparing the magnetic microparticles in athin film fluid formed between two processing surfaces arranged to beopposite to each other so as to be able to approach to and separate fromeach other, at least one of which rotates relative to the other,magnetic microparticles obtained therefrom and a magnetic fluidcontaining the same. The invention can provide monodispersed magneticmicroparticles having a volume-average particle size smaller than thatof the magnetic microparticles obtained by the conventional reactionmethod. Further, the invention can continuously and effectively providemagnetic microparticles and is excellent in production efficiency andcan correspond to mass production. Depending on a necessary amount ofproduction, an apparatus effecting the present invention can bedeveloped in size by using general scale-up concept.

BRIEF DESCRIPTION OF DRAWINGS

FIG. 1(A) is a schematic vertical sectional view showing the concept ofthe apparatus used for carrying out the present invention, FIG. 1(B) isa schematic vertical sectional view showing the concept of anotherembodiment of the apparatus, FIG. 1(C) is a schematic vertical sectionalview showing the concept of still another embodiment of the apparatus,and FIG. 1(D) is a schematic vertical sectional view showing the conceptof still another embodiment of the apparatus.

FIG. 2(A) to FIG. 2(D) each show a schematic vertical sectional viewshowing the concept of still another embodiment of the apparatus shownin FIG. 1.

FIG. 3(A) is a schematic bottom view showing an important part of theapparatus shown in FIG. 2(C), FIG. 3(B) is a schematic bottom viewshowing an important part of another embodiment of the apparatus, FIG.3(C) is a schematic bottom view showing an important part of stillanother embodiment of the apparatus, FIG. 3(D) is a schematic bottomview showing the concept of still another embodiment of the apparatus,FIG. 3(E) is a schematic bottom view showing the concept of stillanother embodiment of the apparatus, and FIG. 3(F) is a schematic bottomview showing the concept of still another embodiment of the apparatus.

FIG. 4(A) to FIG. 4(D) each show a schematic vertical sectional viewshowing the concept of still another embodiment of the apparatus shownin FIG. 1.

FIG. 5(A) to FIG. 5(D) each show a schematic vertical sectional viewshowing the concept of still another embodiment of the apparatus shownin FIG. 1.

FIG. 6(A) to FIG. 6(D) each show a schematic vertical sectional viewshowing the concept of still another embodiment of the apparatus shownin FIG. 1.

FIG. 7(A) to FIG. 7(D) each show a schematic vertical sectional viewshowing the concept of still another embodiment of the apparatus shownin FIG. 1.

FIG. 8(A) to FIG. 8(D) each show a schematic vertical sectional viewshowing the concept of still another embodiment of the apparatus shownin FIG. 1.

FIG. 9(A) to FIG. 9(C) each show a schematic vertical sectional viewshowing the concept of still another embodiment of the apparatus shownin FIG. 1.

FIG. 10(A) to FIG. 10(D) each show a schematic vertical sectional viewshowing the concept of still another embodiment of the apparatus shownin FIG. 1.

FIG. 11(A) and FIG. 11(B) each show a schematic vertical sectional viewshowing the concept of still another embodiment of the apparatus shownin FIG. 1, and FIG. 11(C) is a schematic bottom view showing animportant part of the apparatus shown in FIG. 1(A).

FIG. 12(A) is a schematic vertical sectional view showing an importantpart of another embodiment of a pressure-receiving surface in theapparatus shown in FIG. 1(A), and FIG. 12(B) is a schematic verticalsectional view showing an important part of still another embodiment ofthe apparatus.

FIG. 13 is a schematic vertical sectional view showing an important partof another embodiment of a surface-approaching pressure impartingmechanism 4 in the apparatus shown in FIG. 12(A).

FIG. 14 is a schematic vertical sectional view showing an important partof another embodiment of the apparatus shown in FIG. 12(A), which isprovided with a temperature regulating jacket.

FIG. 15 is a schematic vertical sectional view showing an important partof still another embodiment of the surface-approaching pressureimparting mechanism 4 in the apparatus shown in FIG. 12(A).

FIG. 16(A) is a schematic transverse sectional view showing an importantpart of still another embodiment of the apparatus shown in FIG. 12(A),FIG. 16(B), FIG. 16(C), and FIG. 16(E) to FIG. 16(G) are schematictransverse sectional views each showing an important part of stillanother embodiment of the apparatus, and FIG. 16(D) is a partially cutschematic vertical sectional view showing an important part of stillanother embodiment of the apparatus.

FIG. 17 is a schematic vertical sectional view showing an important partof still another embodiment of the apparatus shown in FIG. 12(A).

FIG. 18(A) is a schematic vertical sectional view showing the concept ofstill another embodiment of the apparatus used for carrying out thepresent invention, and FIG. 18(B) is a partially cut explanatory viewshowing an important part of the apparatus.

FIG. 19(A) is a plane view of a first processing member in the apparatusshown in FIG. 12(A), and FIG. 19(B) is a schematic vertical sectionalview showing an important part thereof.

FIG. 20(A) is a vertical sectional view showing an important part offirst and second processing members in the apparatus shown in FIG.12(A), and FIG. 20(B) is a vertical sectional view showing an importantpart of the first and second processing members with a minute gap.

FIG. 21(A) is a plane view of another embodiment of the first processingmember, and FIG. 21(B) is a vertical sectional view showing an importantpart thereof.

FIG. 22(A) is a plane view of still another embodiment of the firstprocessing member, and FIG. 22(B) is a vertical sectional view showingan important part thereof.

FIG. 23(A) is a plane view of still another embodiment of the firstprocessing member, and FIG. 23(B) is a plane view of still anotherembodiment of the first processing member.

FIG. 24(A), FIG. 24(B), and FIG. 24(C) are diagrams showing embodimentsother than those described above with respect to the method ofseparating a processed material after processing.

FIG. 25 is a schematic vertical sectional view showing outline of theapparatus of the present invention.

FIG. 26(A) is a schematic plane view of the first processing surface inthe apparatus shown in FIG. 25, and FIG. 26(B) is an enlarged viewshowing an important part of the first processing surface in theapparatus shown in FIG. 25.

FIG. 27(A) is a sectional view of the second introduction path, and FIG.27(B) is an enlarged view showing an important part of the processingsurface for explaining the second introduction path.

FIG. 28(A) and FIG. 28(B) are each an enlarged sectional view of animportant part for explaining an inclined surface arranged in theprocessing member.

FIG. 29 is a diagram for explaining a pressure-receiving surfacearranged in the processing member, FIG. 29(A) is a bottom view of thesecond processing member, and FIG. 29(B) is an enlarged sectional viewshowing an important part thereof.

BEST MODE FOR CARRYING OUT THE INVENTION

An apparatus of the same principle as described in JP-A 2004-49957 filedby the present applicant, for example, can be used in the method ofuniform stirring and mixing in a thin film fluid formed betweenprocessing surfaces arranged to be opposite to each other so as to beable to approach to and separate from each other, at least one of whichrotates relative to the other.

Hereinafter, the fluid processing apparatus suitable for carrying outthis method is described.

As shown in FIG. 1(A), this apparatus includes opposing first and secondprocessing members 10 and 20, at least one of which rotates to theother. The opposing surfaces of both the processing members 10 and 20serve as processing surfaces 1 and 2 to process a fluid to be processedtherebetween. The first processing member 10 includes a first processingsurface 1, and the second processing member 20 includes a secondprocessing surface 2.

Both the processing surfaces 1 and 2 are connected to a flow path of thefluid to constitute a part of the flow path of the fluid.

Specifically, this apparatus constitutes flow paths of at least twofluids to be processed and joins the flow paths together.

That is, this apparatus is connected to a flow path of a first fluid toform a part of the flow path of the first fluid and simultaneously formsa part of a flow path of a second fluid different from the first fluid.This apparatus joins both the flow paths together thereby mixing andwhen the mixing is accompanied by reaction, reacting both the fluidsbetween the processing surfaces 1 and 2. In the embodiment shown in FIG.1(A), each of the flow paths is hermetically closed and madeliquid-tight (when the processed fluid is a liquid) or air-tight (whenthe processed fluid is a gas).

Specifically, this apparatus as shown in FIG. 1(A) includes the firstprocessing member 10, the second processing member 20, a first holder 11for holding the first processing member 10, a second holder 21 forholding the second processing member 20, a surface-approaching pressureimparting mechanism 4, a rotation drive member, a first introductionpart d1, a second introduction part d2, a fluid pressure impartingmechanism p1, a second fluid supply part p2, and a case 3.

Illustration of the rotation drive member is omitted.

At least one of the first processing member 10 and the second processingmember 20 is able to approach to and separate from each other, and theprocessing surfaces 1 and 2 are able to approach to and separate fromeach other.

In this embodiment, the second processing member 20 approaches to andseparates from the first processing member 10. On the contrary, thefirst processing member 10 may approach to and separate from the secondprocessing member 20, or both the processing members 10 and 20 mayapproach to and separate from each other.

The second processing member 20 is disposed over the first processingmember 10, and the lower surface of the second processing member 20serves as the second processing surface 2, and the upper surface of thefirst processing member 10 serves as the first processing surface 1.

As shown in FIG. 1(A), the first processing member 10 and the secondprocessing member 20 in this embodiment are circular bodies, that is,rings. Hereinafter, the first processing member 10 is referred to as afirst ring 10, and the second processing member 20 as a second ring 20.

Both the rings 10 and 20 in this embodiment are metallic members having,at one end, a mirror-polished surface, respectively, and theirmirror-polished surfaces are referred to as the first processing surface1 and the second processing surface 2, respectively. That is, the uppersurface of the first ring 10 is mirror-polished as the first processingsurface 1, and the lower surface of the second ring is mirror-polishedas the second processing surface 2.

At least one of the holders can rotate relative to the other holder bythe rotation drive member. In FIG. 1(A), numerical 50 indicates a rotaryshaft of the rotation drive member. The rotation drive member may use anelectric motor. By the rotation drive member, the processing surface ofone ring can rotate relative to the processing surface of the otherring.

In this embodiment, the first holder 11 receives drive power on therotary shaft 50 from the rotation drive member and rotates relative tothe second holder 21, whereby the first ring 10 integrated with thefirst holder 11 rotates relative to the second ring 20. Inside the firstring 10, the rotary shaft 50 is disposed in the first holder 11 so as tobe concentric, in a plane, with the center of the circular first ring10.

The first ring 10 rotates centering on the shaft center of the ring 10.The shaft center (not shown) is a virtual line referring to the centralline of the ring 10.

In this embodiment, as described above, the first holder 11 holds thefirst ring 10 such that the first processing surface 1 of the first ring10 is directed upward, and the second holder 21 holds the second ring 20such that the second processing surface 2 of the second ring 20 isdirected downward.

Specifically, the first and second holders 11 and 21 include aring-accepting concave part, respectively. In this embodiment, the firstring 10 is fitted in the ring-accepting part of the first holder 11, andthe first ring 10 is fixed in the ring-accepting part so as not to risefrom, and set in, the ring-accepting part of the first holder 11.

That is, the first processing surface 1 is exposed from the first holder11 and faces the second holder 21.

Examples of the material for the first ring 10 include metal, ceramics,sintered metal, abrasion-resistant steel, metal subjected to hardeningtreatment, and rigid materials subjected to lining, coating or plating.Particularly, the first processing member 10 is preferably formed of alightweight material for rotation. A material for the second ring 20 maybe the same as that for the first ring 10.

On the other hand, the ring-accepting part 41 arranged in the secondholder 21 accepts the processing member 2 of the second ring 20 suchthat the processing member can rise and set.

The ring-accepting part 41 of the second holder 21 is a concave portionfor mainly accepting that side of the second ring 20 opposite to theprocessing surface 2, and this concave portion is a groove which hasbeen formed into a circle when viewed in a plane.

The ring-accepting part 41 is formed larger in size than the second ring20 and accepts the second ring 20 with sufficient clearance betweenitself and the second ring 20.

By this clearance, the second ring 20 in the ring-accepting part 41 canbe displaced not only in the axial direction of the circularring-accepting part 41 but also in a direction perpendicular to theaxial direction. In other words, the second ring 20 can, by thisclearance, be displaced relative to the ring-accepting part 41 to makethe central line of the ring 20 unparallel to the axial direction of thering-accepting part 41.

Hereinafter, that portion of the second holder 21 which is surrounded bythe second ring 20 is referred to as a central portion 22.

In other words, the second ring 20 is displaceably accepted within thering-accepting part 41 not only in the thrust direction of thering-accepting part 41, that is, in the direction in which the ring 20rises from and sets in the part 41, but also in the decenteringdirection of the ring 20 from the center of the ring-accepting part 41.Further, the second ring 20 is accepted in the ring-accepting part 41such that the ring 20 can be displaced (i.e. run-out) to vary the widthbetween itself upon rising or setting and the ring-accepting part 41, ateach position in the circumferential direction of the ring 20.

The second ring 20, while maintaining the degree of its move in theabove three directions, that is, the axial direction, decenteringdirection and run-out direction of the second ring 20 relative to thering-accepting part 41, is held on the second holder 21 so as not tofollow the rotation of the first ring 10. For this purpose, suitableunevenness (not shown) for regulating rotation in the circumferentialdirection of the ring-accepting part 41 may be arranged both in thering-accepting part 41 and in the second ring 20. However, theunevenness should not deteriorate displacement in the degree of its movein the three directions.

The surface-approaching pressure imparting mechanism 4 supplies theprocessing members with force exerted in the direction of approachingthe first processing surface 1 and the second processing surface 2 eachother. In this embodiment, the surface-approaching pressure impartingmechanism 4 is disposed in the second holder 21 and biases the secondring 20 toward the first ring 10.

The surface-approaching pressure imparting mechanism 4 uniformly biaseseach position in the circumferential direction of the second ring 20,that is, each position of the processing surface 2, toward the firstring 10. A specific structure of the surface-approaching pressureimparting mechanism 4 will be described later.

As shown in FIG. 1(A), the case 3 is arranged outside the outercircumferential surfaces of both the rings 10 and 20, and accepts aproduct formed between the processing surfaces 1 and 2 and discharged tothe outside of both the rings 10 and 20. As shown in FIG. 1(A), the case3 is a liquid-tight container for accepting the first holder 10 and thesecond holder 20. However, the second holder 20 may be that which as apart of the case, is integrally formed with the case 3.

As described above, the second holder 21 whether formed as a part of thecase 3 or formed separately from the case 3 is not movable so as toinfluence the distance between both the rings 10 and 20, that is, thedistance between the processing surfaces 1 and 2. In other words, thesecond holder 21 does not influence the distance between the processingsurfaces 1 and 2.

The case 3 is provided with an outlet 32 for discharging a product tothe outside of the case 3.

The first introduction part d1 supplies a first fluid to the spacebetween the processing surfaces 1 and 2.

The fluid pressure imparting mechanism p1 is connected directly orindirectly to the first introduction part d1 to impart fluid pressure tothe first processed fluid. A compressor or a pump can be used in thefluid pressure imparting mechanism p1.

In this embodiment, the first introduction part d1 is a fluid patharranged inside the central portion 22 of the second holder 21, and oneend of the first introduction part d1 is open at the central position ofa circle, when viewed in a plane, of the second ring 20 on the secondholder 21. The other end of the first introduction part d1 is connectedto the fluid pressure imparting mechanism p1 outside the second holder20, that is, outside the case 3.

The second introduction part d2 supplies a second fluid to be mixed withthe first fluid to the space between the processing surfaces 1 and 2. Inthis embodiment, the second introduction part is a fluid passagearranged inside the second ring 20, and one end of the secondintroduction part is open at the side of the second processing surface2, and a second fluid-feeding part p2 is connected to the other end.

A compressor or a pump can be used in the second fluid-feeding part p2.

The first processed fluid pressurized with the fluid pressure impartingmechanism p1 is introduced from the first introduction part d1 to thespace between the rings 10 and 20 and will pass through the spacebetween the first processing surface 1 and the second processing surface2 to the outside of the rings 10 and 20.

At this time, the second ring 20 receiving the supply pressure of thefirst fluid stands against the bias of the surface-approaching pressureimparting mechanism 4, thereby receding from the first ring 10 andmaking a minute space between the processing surfaces. The space betweenboth the processing surfaces 1 and 2 by approach and separation of thesurfaces 1 and 2 will be described in detail later.

A second fluid is supplied from the second introduction part d2 to thespace between the processing surfaces 1 and 2, flows into the firstfluid, and is subjected to a mixing (reaction) promoted by rotation ofthe processing surface. Then, a reaction product formed by the mixing(reaction) of both the fluids is discharged from the space between theprocessing surfaces 1 and 2 to the outside of the rings 10 and 20. Theproduct discharged to the outside of the rings 10 and 20 is dischargedfinally through the outlet of the case to the outside of the case(self-discharge).

The mixing and reaction (when the mixing is accompanied by reaction) ofthe processed fluid are effected between the first processing surface 1and the second processing surface 2 by rotation, relative to the secondprocessing member 20, of the first processing member 10 with the drivemember 5.

Between the first and second processing surfaces 1 and 2, a regiondownstream from an opening m2 of the second introduction part d2 servesas a processing chamber where the first and second processed fluids aremixed with each other. Specifically, as shown in FIG. 11(C) illustratinga bottom face of the second ring 20, a region H shown by oblique lines,outside the second opening m2 of the second introduction part in theradial direction r1 of the second ring 20, serves as the processingchamber. Accordingly, this processing chamber is located downstream fromthe openings m1 and m2 of the first introduction part d1 and the secondintroduction part d2 between the processing surfaces 1 and 2.

The first fluid introduced from the first opening m1 through a spaceinside the ring into the space between the processing surfaces 1 and 2,and the second fluid introduced from the second opening m2 into thespace between the processing surfaces 1 and 2, are mixed with each otherin the region H serving as the processing chamber, and if the mixing isaccompanied by reaction, both the processed fluids are reacted with eachother. The fluid will, upon receiving supply pressure from the fluidpressure imparting mechanism p1, move through the minute space betweenthe processing surfaces 1 and 2 to the outside of the rings, but becauseof rotation of the first ring 10, the fluid mixed in the reaction regionH does not move linearly from the inside to the outside of the rings inthe radial direction, but moves from the inside to the outside of thering spirally around the rotary shaft of the ring when the processingsurfaces are viewed in a plane. As described above, in the region Hwhere the fluids are thus mixed (reacted), the fluids can move spirallyfrom inside to outside to secure a zone necessary for sufficient mixing(reaction) in the minute space between the processing surfaces 1 and 2,thereby promoting their uniform reaction.

The product formed by the mixing (reaction) becomes a uniform reactionproduct in the minute space between the first processing surface 1 andthe second processing surface 2 and appears as microparticlesparticularly in the case of crystallization or separation.

By the balance among at least the supply pressure applied by the fluidpressure imparting mechanism p1, the bias of the surface-approachingpressure imparting mechanism 4, and the centrifugal force resulting fromrotation of the ring, the distance between the processing surfaces 1 and2 can be balanced to attain a preferable minute space, and further theprocessed fluid receiving the supply pressure applied by the fluidpressure imparting mechanism p1 and the centrifugal force by rotation ofthe ring moves spirally in the minute space between the processingsurfaces 1 and 2, so that their mixing (reaction) is promoted.

The mixing (reaction) is forcedly effected by the supply pressureapplied by the fluid pressure imparting mechanism p1 and the rotation ofthe ring. That is, the mixing (reaction) occurs under forced uniformmixing between the processing surfaces 1 and 2 arranged opposite to eachother so as to be able to approach to and separate from each other, atleast one of which rotates relative to the other.

Accordingly, the crystallization and separation of the product formed bythe reaction can be regulated by relatively easily controllable methodssuch as regulation of supply pressure applied by the fluid pressureimparting mechanism p1 and regulation of the rotation speed of the ring,that is, the number of rotations of the ring.

As described above, this fluid processing apparatus is excellent in thatthe space between the processing surfaces 1 and 2, which can exertinfluence on the size of a product, and the distance in which theprocessed fluid moves in the region H, which can exert influence onformation of a uniform product, can be regulated by the supply pressureand the centrifugal force.

The reaction processing gives not only deposit of the product but alsoliquids. When the product is fine mass such as microparticles, it may bea deposit in the fluid after processing or may be in a dispersion statein which a dispersed phase is present in a continuous phase.

The rotary shaft 50 is not limited to the vertically arranged one andmay be arranged in the horizontal direction or arranged at a slant. Thisis because during processing, the mixing (reaction) occurs in such aminute space between the processing surfaces 1 and 2 that the influenceof gravity can be substantially eliminated.

In FIG. 1(A), the first introduction part d1 extends vertically andcoincides with the shaft center of the second ring 20 in the secondholder 21. However, the first introduction part d1 is not limited to theone having a center coinciding with the shaft center of the second ring20 and may be arranged in other positions in the central portion 22 ofthe second holder 21 as long as the first fluid can be supplied into thespace surrounded by the rings 10 and 20, and the first introduction partd1 may extend obliquely as well as vertically.

A more preferable embodiment of the apparatus is shown in FIG. 12(A). Asshown in this figure, the second processing member 20 has the secondprocessing surface 2 and a pressure-receiving surface 23 which ispositioned inside, and situated next to, the second processing surface2. Hereinafter, the pressure-receiving surface 23 is also referred to asa separation-regulating surface 23. As shown in the figure, theseparation regulating surface 23 is an inclined surface.

As described above, the ring-accepting part 41 is formed in the bottom(i.e. a lower part) of the second holder 21, and the second processingmember 20 is accepted in the ring-accepting part 41. The secondprocessing member 20 is accepted by the second holder 21 so as not to berotated with a baffle (not shown). The second processing surface 2 isexposed from the second holder 21.

In this embodiment, a material to be processed is introduced inside thefirst processing member 10 and the second processing member 20 betweenthe processing surfaces 1 and 2, and the processed material isdischarged to the outside of the first processing member 10 and thesecond processing member 20.

The surface-approaching pressure imparting mechanism 4 presses bypressure the second processing surface 2 against the first processingsurface 1 to make them contacted with or close to each other, andgenerates a fluid film of predetermined thickness by the balance betweenthe surface-approaching pressure and the force, e.g. fluid pressure, ofseparating the processing surfaces 1 and 2 from each other. In otherwords, the distance between the processing surfaces 1 and 2 is kept in apredetermined minute space by the balance between the forces.

Specifically, the surface-approaching pressure imparting mechanism 4 inthis embodiment is comprised of the ring-accepting part 41, aspring-accepting part 42 arranged in the depth of the ring-acceptingpart 41, that is, in the deepest part of the ring-accepting part 41, aspring 43, and an air introduction part 44.

However, the surface-approaching pressure imparting mechanism 4 may bethe one including at least one member selected from the ring acceptingpart 41, the spring-accepting part 42, the spring 43, and the airintroduction part 44.

The ring-accepting part 41 has the second processing member 20 fit intoit with play to enable the second processing member 20 to be displacedvertically deeply or shallowly, that is, vertically in thering-accepting part 41.

One end of the spring 43 is abutted against the depth of thespring-accepting part 42, and the other end of the spring 43 is abuttedagainst the front (i.e. the upper part) of the second processing member20 in the ring-accepting part 41. In FIG. 1, only one spring 43 isshown, but a plurality of springs 44 are preferably used to pressvarious parts of the second processing member 20. This is because as thenumber of the springs 43 increases, pressing pressure can be given moreuniformly to the second processing member 20. Accordingly, several to afew dozen springs 43 comprising a multi-spring type preferably attach tothe second holder 21.

In this embodiment, air can be introduced through the air introductionpart 44 into the ring-accepting part 41. By such introduction of air,air pressure together with pressure by the spring 43 can be given aspressing pressure from the space, as a pressurizing chamber, between thering-accepting part 41 and the second processing member 20 to the secondprocessing member 20. Accordingly, adjusting the pressure of airintroduced through the air introduction part 44 can regulate thesurface-approaching pressure of the second processing surface 2 towardthe first processing surface 1 during operation. A mechanism ofgenerating pressing pressure with another fluid pressure such as oilpressure can be utilized in place of the air introduction part 44utilizing air pressure.

The surface-approaching pressure imparting mechanism 4 not only suppliesand regulates a part of the pressing pressure, that is, thesurface-approaching pressure, but also serves as a displacementregulating mechanism and a buffer mechanism.

Specifically, the surface-approaching pressure imparting mechanism 4 asa displacement regulating mechanism can maintain initial pressingpressure by regulating air pressure against the change in the axialdirection caused by elongation or abrasion at the start of or in theoperation. As described above, the surface-approaching pressureimparting mechanism 4 uses a floating mechanism of maintaining thesecond processing member 20 so as to be displaced, thereby alsofunctioning as a buffer mechanism for micro-vibration or rotationalignment.

Now, the state of the thus constituted processing apparatus during useis described with reference to FIG. 1(A).

At the outset, a first processed fluid is pressurized with the fluidpressure imparting mechanism p1 and introduced through the firstintroduction part d1 into the internal space of the sealed case. On theother hand, the first processing member 10 is rotated with the rotationof the rotary shaft 50 by the rotation drive member. The firstprocessing surface 1 and the second processing surface 2 are therebyrotated relatively with a minute space kept therebetween.

The first processed fluid is formed into a fluid film between theprocessing surfaces 1 and 2 with a minute space kept therebetween, and asecond processed fluid which is introduced through the secondintroduction part d2 flows into the fluid film between the processingsurfaces 1 and 2 to comprise a part of the fluid film. By this, thefirst and second processed fluids are mixed with each other to form aproduct. When the mixing is accompanied by reaction, a uniform reactionof both of the fluids being reacted with each other is promoted to forma reaction product. When the reaction is accompanied by separation,relatively uniform and fine particles can be formed. Even when thereaction is not accompanied by separation, a uniform mixing (uniformreaction when the mixing is accompanied by reaction) can be realized.The separated product may be further finely pulverized by shearingbetween the first processing surface 1 and the second processing surface2 with the rotation of the first processing surface 1. The firstprocessing surface 1 and the second processing surface 2 are regulatedto form a minute space of 1 μm to 1 mm, particularly 1 μm to 10 μm,thereby realizing a uniform mixing (uniform reaction when the mixing isaccompanied by reaction) and enabling formation of superfine particlesof several nm in diameter.

The product is discharged from the processing surfaces 1 and 2 throughan outlet 33 of the case 3 to the outside of the case. The dischargedproduct is atomized in a vacuum or depressurized atmosphere with awell-known decompression device and converted into liquid in theatmosphere to hit each other, then what trickled down in the liquid isable to be collected as degassed liquid.

In this embodiment, the processing apparatus is provided with a case,but may be carried out without a case. For example, a decompression tankfor degassing, that is, a vacuum tank, is arranged, and the processingapparatus may be arranged in this tank. In this case, the outletmentioned above is naturally not arranged in the processing apparatus.

As described above, the first processing surface 1 and the secondprocessing surface 2 can be regulated to form a minute space in theorder of μm which cannot be formed by arranging mechanical clearance.Now, this mechanism is described.

The first processing surface 1 and the second processing surface 2 arecapable of approaching to and separating from each other, andsimultaneously rotate relative to each other. In this example, the firstprocessing surface 1 rotates, and the second processing surface 2approaches to and separates from the first processing surface with astructure capable of moving in the axial direction (floating structure).

In this example, therefore, the position of the second processingsurface 2 in the axial direction is arranged accurately in the order ofμm by the balance between forces, that is, the balance between thesurface-approaching pressure and the separating pressure, therebyestablishing a minute space between the processing surfaces 1 and 2.

As shown in FIG. 12(A), the surface-approaching pressure includes thepressure by air pressure (positive pressure) from the air introductionpart 44 by the surface-approaching pressure imparting mechanism 4, thepressing pressure with the spring 43, and the like.

The embodiments shown in FIG. 13 to FIG. 15 are shown by omitting thesecond introduction part d2 to simplify the drawings. In this respect,these drawings may be assumed to show sections at a position notprovided with the second introduction part d2. In the figures, U and Sshow upward and downward directions respectively.

On the other hand, the separating force include the fluid pressureacting on the pressure-receiving surface at the separating side, thatis, on the second processing surface 2 and the separation regulatingsurface 23, the centrifugal force resulting from rotation of the firstprocessing member 1, and the negative pressure when negative pressure isapplied to the air introduction part 44.

When the apparatus is washed, the negative pressure applied to the airintroduction part 44 can be increased to significantly separate theprocessing surfaces 1 and 2 from each other, thereby facilitatingwashing.

By the balance among these forces, the second processing surface 2 whilebeing remote by a predetermined minute space from the first processingsurface 1 is stabilized, thereby realizing establishment with accuracyin the order of μm.

The separating force is described in more detail.

With respect to fluid pressure, the second processing member 20 in aclosed flow path receives feeding pressure of a processed fluid, thatis, fluid pressure, from the fluid pressure imparting mechanism p. Inthis case, the surfaces opposite to the first processing surface in theflow path, that is, the second processing surface 2 and the separationregulating surface 23, act as pressure-receiving surfaces at theseparating side, and the fluid pressure is applied to thepressure-receiving surfaces to generate a separating force due to thefluid pressure.

With respect to centrifugal force, the first processing member 10 isrotated at high speed, centrifugal force is applied to the fluid, and apart of this centrifugal force acts as a separating force in thedirection in which the processing surfaces 1 and 2 are separated fromeach other.

When negative pressure is applied from the air introduction part 44 tothe second processing member 20, the negative pressure acts as aseparating force.

In the foregoing description of the present invention, the force ofseparating the first and second processing surfaces 1 and 2 from eachother has been described as a separating force, and the above-mentionedforce is not excluded from the separating force.

By forming a balanced state of the separating force and thesurface-approaching pressure applied by the surface-approaching pressureimparting mechanism 4 via the processed fluid between the processingsurfaces 1 and 2 in the flow path of the closed processed fluid, auniform mixing (uniform reaction when the mixing is accompanied byreaction) is realized between the processing surfaces 1 and 2, andsimultaneously a fluid film suitable for crystallization and separationof microscopic products is formed as described above. In this manner,this apparatus can form a forced fluid film between the processingsurfaces 1 and 2 via which a minute space not achievable with aconventional mechanical apparatus can be kept between the processingsurfaces 1 and 2, and microparticles can be formed highly accurately asthe reaction product.

In other words, the thickness of the fluid film between the processingsurfaces 1 and 2 is regulated as desired by regulating the separatingforce and surface-approaching pressure, thereby realizing a necessaryuniform mixing (uniform reaction when the mixing is accompanied byreaction) to form and process microscopic products. Accordingly, whenthe thickness of the fluid film is to be decreased, thesurface-approaching pressure or separating force may be regulated suchthat the surface-approaching pressure is made relatively higher than theseparating force. When the thickness of the fluid film is to beincreased, the separating force or surface-approaching pressure may beregulated such that the separating force is made relatively higher thanthe surface-approaching pressure.

When the surface-approaching pressure is increased, air pressure, thatis, positive pressure is applied from the air introduction part 44 bythe surface-approaching pressure imparting mechanism 4, or the spring 43is changed to the one having higher pressing pressure, or the number ofthe springs may be increased.

When the separating force is to be increased, the feeding pressure ofthe fluid pressure imparting mechanism p1 is increased, or the area ofthe second processing surface 2 or the separation regulating surface 23is increased, or in addition, the rotation of the second processingmember 20 is regulated to increase centrifugal force or reduce pressurefrom the air introduction part 44. Alternatively, negative pressure maybe applied. The spring 43 shown is a pressing spring that generatespressing pressure in an extending direction, but may be a pulling springthat generates a force in a compressing direction to constitute a partor the whole of the surface-approaching pressure imparting mechanism 4.

When the separating force is to be decreased, the feeding pressure ofthe fluid pressure imparting mechanism p1 is reduced, or the area of thesecond processing surface 2 or the separation regulating surface 23 isreduced, or in addition, the rotation of the second processing member 20is regulated to decrease centrifugal force or increase pressure from theair introduction part 44. Alternatively, negative pressure may bereduced.

Further, properties of a processed fluid, such as viscosity, can beadded as a factor for increasing or decreasing the surface-approachingpressure and separating force, and regulation of such properties of aprocessed fluid can be performed as regulation of the above factor.

In the separating force, the fluid pressure exerted on thepressure-receiving surface at the separating side, that is, the secondprocessing surface 2 and the separation regulating surface 23 isunderstood as a force constituting an opening force in mechanical seal.

In the mechanical seal, the second processing member 20 corresponds to acompression ring, and when fluid pressure is applied to the secondprocessing member 2, the force of separating the second processingmember 2 from the first processing member 1 is regarded as an openingforce.

More specifically, when the pressure-receiving surfaces at a separatingside, that is, the second processing surface 2 and the separationregulating surface 23 only are arranged in the second processing member20 as shown in the first embodiment, all feeding pressure constitutesthe opening force. When a pressure-receiving surface is also arranged atthe backside of the second processing member 20, specifically in thecase of FIG. 12(B) and FIG. 17 described later, the difference betweenthe feeding pressure acting as a separating force and the feedingpressure acting as surface-approaching pressure is the opening force.

Now, other embodiments of the second processing member 20 are describedwith reference to FIG. 12(B).

As shown in FIG. 12(B), an approach regulating surface 24 facing upward,that is, at the other side of the second processing surface 2, isdisposed at the inner periphery of the second processing member 20exposed from the ring-accepting part 41.

That is, the surface-approaching pressure imparting mechanism 4 in thisembodiment is comprised of a ring-accepting part 41, an air introductionpart 44, and the approach regulating surface 24. However, thesurface-approaching pressure imparting mechanism 4 may be one includingat least one member selected from the ring-accepting part 41, thespring-accepting part 42, the spring 43, the air introduction part 44,and the approach regulating surface 24.

The approach regulating surface 24 receives predetermined pressureapplied to a processed fluid to generate a force of approaching thesecond processing surface 2 to the first processing surface 1, therebyfunctioning in feeding surface-approaching pressure as a part of thesurface-approaching pressure imparting mechanism 4. On the other hand,the second processing surface 2 and the separation regulating surface 23receive predetermined pressure applied to a processed fluid to generatea force of separating the second processing surface 2 from the firstprocessing surface 1, thereby functioning in feeding a part of theseparating force.

The approach regulating surface 24, the second processing surface 2 andthe separation regulating surface 23 are pressure-receiving surfacesreceiving feeding pressure of the processed fluid, and depending on itsdirection, exhibits different actions, that is, generation of thesurface-approaching pressure and generation of a separating force.

The ratio (area ratio A1/A2) of a projected area A1 of the approachregulating surface 24 projected on a virtual plane perpendicular to thedirection of approaching and separating the processing surfaces, thatis, in the direction of rising and setting of the second ring 20, to atotal area A2 of the projected area of the second processing surface 2and the separating side pressure-receiving surface 23 of the secondprocessing member 20 projected on the virtual plane is called balanceratio K which is important for regulation of the opening force.

Both the top of the approach regulating surface 24 and the top of theseparating side pressure-receiving surface 23 are defined by the innerperiphery 25 of the circular second regulating part 20, that is, by topline L1. Accordingly, the balance ratio K is regulated for deciding theplace where base line L2 of the approach regulating surface 24 is to beplaced.

That is, in this embodiment, when the feeding pressure of the processedfluid is utilized as an opening force, the total projected area of thesecond processing surface 2 and the separation regulating surface 23 ismade larger than the projected area of the approach regulating surface24, thereby generating an opening force in accordance with the arearatio.

The opening force can be regulated by the pressure of the processedfluid, that is, the fluid pressure, by changing the balance line, thatis, by changing the area A1 of the approach regulating surface 24.

Sliding surface actual surface pressure P, that is, the fluid pressureout of the surface-approaching pressure, is calculated according to thefollowing equation:P=P1×(K−k)+Ps

wherein P1 represents the pressure of a processed fluid, that is, fluidpressure, K represents the balance ratio, k represents an opening forcecoefficient, and Ps represents a spring and back pressure.

By regulating this balance line to regulate the sliding surface actualsurface pressure P, the space between the processing surfaces 1 and 2 isformed as a desired minute space, thereby forming a fluid film of aprocessed fluid to make the product minute and effecting uniform mixing(reaction) processing.

Usually, as the thickness of a fluid film between the processingsurfaces 1 and 2 is decreased, the product can be made finer. On theother hand, as the thickness of the fluid film is increased, processingbecomes rough and the throughput per unit time is increased. Byregulating the sliding surface actual surface pressure P on the slidingsurface, the space between the processing surfaces 1 and 2 can beregulated to realize the desired uniform mixing (uniform reaction whenthe mixing is accompanied by reaction) and to obtain the minute product.Hereinafter, the sliding surface actual surface pressure P is referredto as surface pressure P.

From this relation, it is concluded that when the product is to be madecoarse, the balance ratio may be decreased, the surface pressure P maybe decreased, the space may be increased and the thickness of the filmmay be increased. On the other hand, when the product is to be madefiner, the balance ratio K may be increased, the surface pressure P maybe increased, the space may be decreased and the thickness of the filmmay be decreased.

As a part of the surface-approaching pressure imparting mechanism 4, theapproach regulating surface 24 is formed, and at the position of thebalance line, the surface-approaching pressure may be regulated, thatis, the space between the processing surfaces may be regulated.

As described above, the space is regulated in consideration of thepressing pressure of the spring 43 and the air pressure of the airintroduction part 44. Regulation of the fluid pressure, that is, thefeeding pressure of the processed fluid, and regulation of the rotationof the first processing member 10 for regulating centrifugal force, thatis, the rotation of the first holder 11, are also important factors toregulate the space.

As described above, this apparatus is constituted such that for thesecond processing member 20 and the first processing member 10 thatrotates relative to the second processing member 20, a predeterminedfluid film is formed between the processing surfaces by pressure balanceamong the feeding pressure of the processed fluid, the rotationcentrifugal force, and the surface-approaching pressure. At least one ofthe rings is formed in a floating structure by which alignment such asrun-out is absorbed to eliminate the risk of abrasion and the like.

The embodiment shown in FIG. 1(A) also applies to the embodiment in FIG.12(B) except that the regulating surface is arranged.

The embodiment shown in FIG. 12(B) can be carried out without arrangingthe pressure-receiving surface 23 on the separating side, as shown inFIG. 17.

When the approach regulating surface 24 is arranged as shown in theembodiment shown in FIG. 12(B) and FIG. 17, the area A1 of the approachregulating surface 24 is made larger than the area A2, whereby all ofthe predetermined pressure exerted on the processed fluid functions assurface-approaching pressure, without generating an opening force. Thisarrangement is also possible, and in this case, both the processingsurfaces 1 and 2 can be balanced by increasing other separating force.

With the area ratio described above, the force acting in the directionof separating the second processing surface 2 from the first processingsurface 1 is fixed as the resultant force exerted by the fluid.

In this embodiment, as described above, the number of the springs 43 ispreferably larger in order to impart uniform stress on the slidingsurface, that is, the processing surface. However, the spring 43 may bea single coil-type spring as shown in FIG. 13. As shown in the figure,this spring is a single coil spring having a center concentric with thecircular second processing member 20.

The space between the second processing member 20 and the second holder21 is sealed air-tightly with methods well known in the art.

As shown in FIG. 14, the second holder 21 is provided with a temperatureregulation jacket 46 capable of regulating the temperature of the secondprocessing member 20 by cooling or heating. Numerical 3 in FIG. 14 isthe above-mentioned case, and the case 3 is also provided with a jacket35 for the same purpose of temperature regulation.

The temperature regulation jacket 46 for the second holder 21 is awater-circulating space formed at a side of the ring-accepting part 41and communicates with paths 47 and 48 leading to the outside of thesecond holder 21. One of the paths 47 and 48 introduces a cooling orheating medium into the temperature regulation jacket 46, and the otherdischarges the medium.

The temperature regulation jacket 35 for the case 3 is a path forpassing heating water or cooling water, which is arranged between outerperiphery of the case 3 and a covering part 34 for covering the outerperiphery of the case 3.

In this embodiment, the second holder 21 and the case 3 are providedwith the temperature regulation jacket, but the first holder 11 can alsobe provided with such a jacket.

As a part of the surface-approaching pressure imparting mechanism 4, acylinder mechanism 7 shown in FIG. 15 may be arranged besides themembers described above.

The cylinder mechanism 7 includes a cylinder space 70 arranged in thesecond holder 21, a communicating part 71 that communicates the cylinderspace 70 with the ring-accepting part 41, a piston 72 that is acceptedin the cylinder space 70 and connected via the communication part 71 tothe second processing member 20, a first nozzle 73 that communicates tothe upper part of the cylinder space 70, a second nozzle 74 in a lowerpart of the cylinder space 70, and a pressing body 75 such as springbetween the upper part of the cylinder space 70 and the piston 72.

The piston 72 can slide vertically in the cylinder space 70, and thesecond processing member 20 can slide vertically with sliding of thepiston 72, to change the gap between the first processing surface 1 andthe second processing surface 2.

Although not shown in the figure, specifically, a pressure source suchas a compressor is connected to the first nozzle 73, and air pressure,that is, positive pressure is applied from the first nozzle 73 to theupper part of the piston 72 in the cylinder space 70, thereby slidingthe piston 72 downward, to allow the second processing member 20 tonarrow the gap between the first and second processing surfaces 1 and 2.Although not shown in the figure, a pressure source such as a compressoris connected to the second nozzle 74, and air pressure, that is,positive pressure is applied from the second nozzle 74 to the lower partof the piston 72 in the cylinder space 70, thereby sliding the piston 72upward, to allow the second processing member 20 to widen the gapbetween the first and second processing surfaces 1 and 2, that is, toenable it to move in the direction of opening the gap. In this manner,the surface-approaching pressure can be regulated by air pressure withthe nozzles 73 and 74.

Even if there is a space between the upper part of the second processingmember 20 in the ring-accepting part 41 and the uppermost part of thering-accepting part 41, the piston 7 is arranged so as to abut againstan uppermost part 70 a of the cylinder space 70, whereby the uppermostpart 70 a of the cylinder space 70 defines the upper limit of the widthof the gap between the processing surfaces 1 and 2. That is, the piston7 and the uppermost part 70 a of the cylinder space 70 function as aseparation preventing part for preventing the separation of theprocessing surfaces 1 and 2 from each other, in other words, function inregulating the maximum opening of the gap between both the processingsurfaces 1 and 2.

Even if the processing surfaces 1 and 2 do not abut on each other, thepiston 7 is arranged so as to abut against a lowermost part 70 b of thecylinder space 70, whereby the lowermost part 70 b of the cylinder space70 defines the lower limit of the width of the gap between theprocessing surfaces 1 and 2. That is, the piston 7 and the lowermostpart 70 b of the cylinder space 70 function as an approach preventingpart for preventing the approaching of the processing surfaces 1 and 2each other, in other words, function in regulating the minimum openingof the gap between both the processing surfaces 1 and 2.

In this manner, the maximum and minimum openings of the gap areregulated, while a distance z1 between the piston 7 and the uppermostpart 70 a of the cylinder space 70, in other words, a distance z2between the piston 7 and the lowermost part 70 b of the cylinder space70, is regulated with air pressure by the nozzles 73 and 74.

The nozzles 73 and 74 may be connected to a different pressure sourcerespectively, and further may be connected to a single pressure sourcealternatively or switched the connections to the sources.

The pressure source may be a source applying positive or negativepressure. When a negative pressure source such as a vacuum is connectedto the nozzles 73 and 74, the action described above goes to thecontrary.

In place of the other surface-approaching pressure imparting mechanism 4or as a part of the surface-approaching pressure imparting mechanism 4,such cylinder mechanism 7 is provided to set the pressure of thepressure source connected to the nozzle 73 and 74, and the distances z1and z2 according to the viscosity and properties of the fluid to beprocessed in a fashion to bring the thickness value of fluid film of thefluid to a desired level under a shear force to realize a uniform mixing(uniform reaction when the mixing is accompanied by reaction) forforming fine particles. Particularly, such cylinder mechanism 7 can beused to increase the reliability of cleaning and sterilization byforcing the sliding part open and close during cleaning and steamsterilization.

As shown in FIG. 16(A) to FIG. 16(C), the first processing surface 1 ofthe first processing member 10 may be provided with groove-likedepressions 13 . . . 13 extending in the radial direction, that is, inthe direction from the center to the outside of the first processingmember 10. In this case, as shown in FIG. 16(A), the depressions 13 . .. 13 can be curved or spirally elongated on the first processing surface1, and as shown in FIG. 16(B), the individual depression 13 may be bentat a right angle, or as shown in FIG. 16(C), the depressions 13 . . . 13may extend straight radially.

As shown in FIG. 16(D), the depressions 13 in FIG. 16(A) to FIG. 16(C)preferably deepen gradually in the direction toward the center of thefirst processing surface 1. The groove-like depressions 13 may continuein sequence or intermittence.

Formation of such depression 13 may correspond to the increase ofdelivery of the processed fluid or to the decrease of calorific value,while having effects of cavitation control and fluid bearing.

In the embodiments shown in FIG. 16, the depressions 13 are formed onthe first processing surface 1, but may be formed on the secondprocessing surface 2 or may be formed on both the first and secondprocessing surfaces 1 and 2.

When the depressions 13 or tapered sections are not provided on theprocessing surface or are arranged unevenly on a part of the processingsurface, the influence exerted by the surface roughness of theprocessing surfaces 1 and 2 on the processed fluid is greater than thatby the above depressions 13. In this case, the surface roughness shouldbe reduced, that is, the surface should be fine-textured, as theparticle size of the processed fluid are to be decreased. Particularly,regarding the surface roughness of the processing surface, the mirrorsurface, that is, a surface subjected to mirror polishing isadvantageous in realizing uniform mixing (uniform reaction when themixing is accompanied by reaction) for the purpose of uniform mixing(reaction), and in realizing crystallization and separation of finemonodisperse products for the purpose of obtaining microparticles.

In the embodiments shown in FIG. 12 to FIG. 17, structures other thanthose particularly shown are the same as in the embodiments shown inFIG. 1(A) or FIG. 11(C).

In the embodiments described above, the case is closed. Alternatively,the first processing member 10 and the second processing member 20 maybe closed inside but may be open outside. That is, the flow path issealed until the processed fluid has passed through the space betweenthe first processing surface 1 and the second processing surface 2, toallow the processed fluid to receive the feeding pressure, but after thepassing, the flow path may be opened so that the processed fluid afterprocessing does not receive feeding pressure.

The fluid pressure imparting mechanism p1 preferably uses a compressoras a pressure device described above, but if predetermined pressure canalways be applied to the processed fluid, another means may be used. Forexample, the own weight of the processed fluid can be used to applycertain pressure constantly to the processed fluid.

In summary, the processing apparatus in each embodiment described aboveis characterized in that predetermined pressure is applied to a fluid tobe processed, at least two processing surfaces, that is, a firstprocessing surface 1 and a second processing surface 2 capable ofapproaching to and separating from each other are connected to a sealedflow path through which the processed fluid receiving the predeterminedpressure flows, a surface-approaching pressure of approaching theprocessing surfaces 1 and 2 each other is applied to rotate the firstprocessing surface 1 and the second processing surface 2 relative toeach other, thereby allowing a fluid film used for seal in mechanicalseal to be generated out of the processed fluid, and the fluid film isleaked out consciously (without using the fluid film as seal) frombetween the first processing surface 1 and the second processing surface2, contrary to mechanical seal, whereby mixing (reaction) processing isrealized between the processed fluid formed into a film between thesurfaces 1 and 2, and the product is recovered.

By this epoch-making method, the space between the processing surfaces 1and 2 can be regulated in the range of 1 μm to 1 mm, particularly 1 μmto 10 μm.

In the embodiment described above, a flow path for a sealed fluid isconstituted in the apparatus, and the processed fluid is pressurizedwith the fluid pressure imparting mechanism p1 arranged at the side ofthe introduction part (for the first processing fluid) in the processingapparatus.

Alternatively, the flow path for the processed fluid may be openedwithout pressurization with the fluid pressure imparting mechanism p1.

One embodiment of the processing apparatus is shown in FIG. 18 to FIG.20. The processing apparatus illustrated in this embodiment is anapparatus including a degassing mechanism, that is, a mechanism ofremoving a liquid from the formed processed product thereby finallysecuring objective solids (crystals) only.

FIG. 18(A) is a schematic vertical sectional view of the processingapparatus, and FIG. 18(B) is its partially cut enlarged sectional view.FIG. 19 is a plane view of the first processing member 1 arranged in theprocessing apparatus in FIG. 18. FIG. 20 is a partially cut schematicvertical sectional view showing an important part of the first andsecond processing members 1 and 2 in the processing apparatus.

As described above, the apparatus shown in FIG. 18 to FIG. 20 is the oneinto which a fluid as the object of processing, that is, a processedfluid, or a fluid carrying the object of processing, is to be introducedat atmospheric pressure.

In FIG. 18(B) and FIG. 20, the second introduction part d2 is omittedfor simplicity of the drawing (these drawings can be regarded as showinga section at the position where the second introduction part d2 is notarranged).

As shown in FIG. 18(A), this fluid processing apparatus includes amixing apparatus G and a decompression pump Q. This mixing apparatus Gincludes a first processing member 101 as a rotating member, a firstholder 111 for holding the processing member 101, a second processingmember 102 that is a member fixed to the case, a second holder 121having the second processing member 102 fixed thereto, a bias mechanism103, a dynamical pressure generating mechanism 104 (FIG. 19(A)), a drivepart which rotates the first processing member 101 with the first holder111, a housing 106, a first introduction part d1 which supplies(introduces) a first processed fluid, and a discharge part 108 thatdischarges the fluid to the decompression pump Q. The drive part is notshown.

The first processing member 101 and the second processing member 102 arecylindrical bodies that are hollow in the center. The processing members101 and 102 are members wherein the bottoms of the processing members101 and 102 in a cylindrical form are processing surfaces 110 and 120respectively.

The processing surfaces 110 and 120 have a mirror-polished flat part. Inthis embodiment, the processing surface 120 of the second processingmember 102 is a flat surface subjected as a whole to mirror polishing.The processing surface 110 of the first processing member 101 is a flatsurface as a whole like the second processing member 102, but has aplurality of grooves 112 . . . 112 in the flat surface as shown in FIG.19(A). The grooves 112 . . . 112 while centering on the first processingmember 101 in a cylindrical form extend radially toward the outerperiphery of the cylinder.

The processing surfaces 110 and 120 of the first and second processingmembers 101 and 102 are mirror-polished such that the surface roughnessRa comes to be in the range of 0.01 μm to 1.0 μm. By this mirrorpolishing, Ra is regulated preferably in the range of 0.03 μm to 0.3 μm.

The material for the processing members 101 and 102 is one which isrigid and capable of mirror polishing. The rigidity of the processingmembers 101 and 102 is preferably at least 1500 or more in terms ofVickers hardness. A material having a low linear expansion coefficientor high thermal conductance is preferably used. This is because when thedifference in coefficient of expansion between a part which generatesheat upon processing and other parts is high, distortion is generatedand securement of suitable clearance is influenced.

As the material for the processing members 101 and 102, it is preferableto use particularly SIC, that is, silicon carbide, SIC having a Vickershardness of 2000 to 2500, SIC having a Vickers hardness of 3000 to 4000coated thereon with DLC (diamond-like carbon), WC, that is, tungstencarbide having a Vickers hardness of 1800, WC coated thereon with DLC,and boron ceramics represented by ZrB₂, BTC and B₄C having a Vickershardness of 4000 to 5000.

The housing 106 shown in FIG. 18, the bottom of which is not shownthough, is a cylinder with a bottom, and the upper part thereof iscovered with the second holder 121. The second holder 121 has the secondprocessing member 102 fixed to the lower surface thereof, and theintroduction part d1 is arranged in the upper part thereof. Theintroduction part d1 is provided with a hopper 170 for introducing afluid or a processed material from the outside.

Although not shown in the figure, the drive part includes a power sourcesuch as a motor and a shaft 50 that rotates by receiving power from thepower source.

As shown in FIG. 18(A), the shaft 50 is arranged in the housing 106 andextends vertically. Then, the first holder 111 is arranged on the top ofthe shaft 50. The first holder 111 is to hold the first processingmember 101 and is arranged on the shaft 50 as described above, therebyallowing the processing surface 110 of the first processing member 101to correspond to the processing surface 120 of the second processingmember 102.

The first holder 111 is a cylindrical body, and the first processingmember 101 is fixed on the center of the upper surface. The firstprocessing member 101 is fixed so as to be integrated with the firstholder 111, and does not change its position relative to the firstholder 111.

On the other hand, a receiving depression 124 for receiving the secondprocessing member 102 is formed on the center of the upper surface ofthe second holder 121.

The receiving depression 124 has a circular cross-section. The secondprocessing member 102 is accepted in the cylindrical receivingdepression 124 so as to be concentric with the receiving depression 124.

The structure of the receiving depression 124 is similar to that in theembodiment as shown in FIG. 1(A) (the first processing member 101corresponds to the first ring 10, the first holder 111 to the firstholder 11, the second processing member 102 to the second ring 20, andthe second holder 121 to the second holder 21).

Then, the second holder 121 is provided with the bias mechanism 103. Thebias mechanism 103 preferably uses an elastic body such as spring. Thebias mechanism 103 corresponds to the surface-approaching pressureimparting mechanism 4 in FIG. 1(A) and has the same structure. That is,the bias mechanism 103 presses that side (bottom) of the secondprocessing member 102 which is opposite to the processing surface 120and biases each position of the second processing member 102 uniformlydownward to the first processing member 101.

On the other hand, the inner diameter of the receiving depression 124 ismade larger than the outer diameter of the second processing member 102,so that when arranged concentrically as described above, a gap t1 is setbetween outer periphery 102 b of the second processing member 102 andinner periphery of the receiving depression 124, as shown in FIG. 18(B).

Similarly, a gap t2 is set between inner periphery 102 a of the secondprocessing member 102 and outer periphery of the central portion 22 ofthe receiving depression 124, as shown in FIG. 18(B).

The gaps t1 and t2 are those for absorbing vibration and eccentricbehavior and are set to be in a size to secure operational dimensions ormore and to enable sealing. For example, when the diameter of the firstprocessing member 101 is 100 mm to 400 mm, the gaps t1 and t2 arepreferably 0.05 mm to 0.3 mm, respectively.

The first holder 111 is fixed integrally with the shaft 50 and rotatedwith the shaft 50. The second processing member 102 is not rotatedrelative to the second holder 121 by a baffle (not shown). However, forsecuring 0.1 μm to 10 μm clearance necessary for processing, that is,the minute gap t between the processing surfaces 110 and 120 as shown inFIG. 20(B), a gap t3 is, as shown in FIG. 18(B), arranged between thebottom of the receiving depression 124, that is, the top part, and thesurface facing a top part 124 a of the second processing member 102,that is, the upper part. The gap t3 is established in consideration ofthe clearance and the vibration and elongation of the shaft 50.

As described above, by the provision of the gaps t1 to t3, the firstprocessing member 101, as shown in FIG. 18(B), can move not only in thedirection z1 of approaching to and separating from the second processingmember 102, but also relative to the center and direction of theprocessing surface 110, that is, relative to the direction z2.

That is, in this embodiment, the bias mechanism 103 and the gaps t1 tot3 constitute a floating mechanism, and by this floating mechanism, thecenter and inclination of at least the second processing member 102 aremade variable in the small range of several μm to several mm. Therun-out and expansion of the rotary shaft and the surface vibration andvibration of the first processing member 101 are absorbed.

The groove 112 on the processing surface 110 of the first processingmember 101 is described in more detail. The rear end of the groove 112reaches the inner periphery 101 a of the first processing member 101,and its top is elongated toward the outside y of the first processingmember 101, that is, toward the outer periphery. As shown in FIG. 19(A),the sectional area of the groove 112 is gradually decreased in thedirection from the center x of the circular first processing member 101to the outside y of the first processing member 101, that is, toward theouter periphery.

The distance w1 of the left and right sides 112 a and 112 b of thegroove 112 is decreased in the direction from the center x of the firstprocessing member 101 to the outside y of the first processing member101, that is, toward the outer periphery. As shown in FIG. 19(B), thedepth w2 of the groove 112 is decreased in the direction from the centerx of the first processing member 101 to the outside y of the firstprocessing member 101, that is, toward the outer periphery. That is, thebottom 112 c of the groove 112 is decreased in depth in the directionfrom the center x of the first processing member 101 to the outside y ofthe first processing member 101, that is, toward the outer periphery.

As described above, the groove 112 is gradually decreased both in widthand depth toward the outside y, that is, toward the outer periphery, andits sectional area is gradually decreased toward the outside y. Then,the top of the groove 112, that is, the y side, is a dead end. That is,the top of the groove 112, that is, the y side does not reach the outerperiphery 101 b of the first processing member 101, and an outer flatsurface 113 is interposed between the top of the groove 112 and theouter periphery 101 b. The outer flat surface 113 is a part of theprocessing surface 110.

In the embodiment shown in FIG. 19, the left and right sides 112 a and112 b and the bottom 112 c of the groove 112 constitute a flow pathlimiting part. This flow path limiting part, the flat part around thegroove 112 of the first processing member 101, and the flat part of thesecond processing member 102 constitute the dynamical pressuregenerating mechanism 104.

However, only one of the width and depth of the groove 112 may beconstituted as described above to decrease the sectional area.

While the first processing member 101 rotates, the dynamical pressuregenerating mechanism 104 generates a force in the direction ofseparating the processing members 101 and 102 from each other to securea desired minute space between the processing members 101 and 102 by afluid passing through the space between the processing members 101 and102. By generation of such dynamical pressure, a 0.1 μm to 10 μm minutespace can be generated between the processing surfaces 110 and 120. Aminute space like that can be regulated and selected depending on theobject of processing, but is preferably 1 μm to 6 μm, more preferably 1μm to 2 μm. This apparatus can realize a uniform mixing (uniformreaction when the mixing is accompanied by reaction) and formmicroparticles by the minute space, which are not achieved in the priorart.

The grooves 112 . . . 112 may extend straight from the center x to theoutside y. In this embodiment, however, as shown in FIG. 19(A), thegrooves 112 are curved to extend such that with respect to a rotationdirection r of the first processing member 101, the center x of thegroove 112 is positioned in front of the outside y of the groove 112.

In this manner, the grooves 112 . . . 112 are curved to extend so thatthe separation force by the dynamical pressure generating mechanism 104can be effectively generated.

Then, the working of this apparatus is described.

As shown in FIG. 18(A), a first processed fluid R which has beenintroduced from a hopper 170 and has passed through the firstintroduction part d1, passes through the hollow part of the circularsecond processing member 102, and the fluid that has received thecentrifugal force resulting from rotation of the first processing member101 enters the space between the processing members 101 and 102, anduniform mixing (reaction) and, in any case, generation of microparticlesare effected and processed between the processing surface 110 of therotating first processing member 101 and the processing surface 120 ofthe second processing member 102, then exits from the processing members101 and 102 and is then discharged from the discharge part 108 to theside of the decompression pump Q (hereinafter, the first processed fluidR is referred to simply as a fluid R, if necessary).

In the foregoing description, the fluid R that has entered the hollowpart of the circular second processing member 102 first enters thegroove 112 of the rotating first processing member 101 as shown in FIG.20(A). On the other hand, the processing surfaces 110 and 120 that aremirror-polished flat parts are kept airtight even by passing a gas suchas air or nitrogen. Accordingly, even if the centrifugal force byrotation is received, the fluid R cannot enter through the groove 112into the space between the processing surfaces 110 and 120 that arepushed against each other by the bias mechanism 103. However, the fluidR gradually runs against both the sides 112 a and 112 b and the bottom112 c of the groove 112 formed as a flow path limiting part to generatedynamical pressure acting in the direction of separating the processingsurfaces 110 and 120 from each other. As shown in FIG. 20(B), the fluidR can thereby exude from the groove 112 to the flat surface, to secure aminute gap t, that is, clearance, between the processing surfaces 110and 120. Then, a uniform mixing (reaction) and, in any cases, generationof microparticles are effected and processed between the mirror-polishedflat surfaces. The groove 112 has been curved so that the centrifugalforce is applied more accurately to the fluid to make generation ofdynamical pressure more effectively.

In this manner, the fluid processing apparatus can secure a minute anduniform gap, that is, clearance, between the mirror surfaces, that is,the processing surfaces 110 and 120, by the balance between thedynamical pressure and the bias force by the bias mechanism 103. By thestructure described above, the minute gap can be as superfine as 1 μm orless.

By utilizing the floating mechanism, the automatic regulation ofalignment between the processing surfaces 110 and 120 becomes possible,and the clearance in each position between the processing surfaces 110and 120 can be prevented from varying against physical deformation ofeach part by rotation or generated heat, and the minute gap in eachposition can be maintained.

In the embodiment described above, the floating mechanism is a mechanismarranged for the second holder 121 only. Alternatively, the floatingmechanism can be arranged in the first holder 111 instead of, ortogether with, the second holder 121.

Other embodiments of the groove 112 are shown in FIG. 21 to FIG. 23.

As shown in FIG. 21(A) and FIG. 21(B), the groove 112 can be provided atthe top with a flat wall surface 112 d as a part of the flow pathlimiting part. In the embodiment shown in FIG. 21, a step 112 e isarranged between the first wall surface 112 d and the inner periphery101 a in the bottom 112 c, and the step 112 e also constitutes a part ofthe flow path limiting part.

As shown in FIG. 22(A) and FIG. 22(B), the groove 112 includes aplurality of branches 112 f . . . 112 f, and each branch 112 f narrowsits width thereby being provided with a flow path limiting part.

With respect to the embodiments in FIG. 21 and FIG. 22, structures otherthan those particularly shown are similar to those of embodiments asshown in FIG. 1(A), FIG. 11(C), and FIG. 18 to FIG. 20.

In the embodiments described above, at least either the width or depthof the groove 112 is gradually decreased in size in the direction frominside to outside the first processing member 101, thereby constitutinga flow path limiting part. Alternatively, as shown in FIG. 23(A) or FIG.23(B), the groove 112 can be provided with a termination surface 112 fwithout changing the width and depth of the groove 112, and thetermination surface 112 f of the groove 112 can serve as a flow pathlimiting part. As shown in the embodiments in FIG. 19, FIG. 21 and FIG.22, the width and depth of the groove 112 can be changed as describedabove thereby slanting the bottom and both sides of the groove 112, sothat the slanted surface serves as a pressure-receiving part toward thefluid to generate dynamical pressure. In the embodiment shown in FIG.23(A) and FIG. 23(B), on the other hand, the termination surface of thegroove 112 serves as a pressure-receiving part toward the fluid togenerate dynamical pressure.

In the embodiment shown in FIG. 23(A) and FIG. 23(B), at least one ofthe width and depth of the groove 112 may also be gradually decreased insize.

The structure of the groove 112 is not limited to the one shown in FIG.19 and FIG. 21 to FIG. 23 and can be provided with a flow path limitingpart having other shapes.

For example, in the embodiments shown in FIG. 19 and FIG. 21 to FIG. 23,the groove 112 does not penetrate to the outer side of the firstprocessing member 101. That is, there is the outer flat surface 113between the outer periphery of the first processing member 101 and thegroove 112. However, the structure of the groove 112 is not limited tosuch embodiment, and the groove 112 may reach the outer periphery of thefirst processing member 101 as long as the dynamical pressure can begenerated.

For example, in the case of the first processing member 101 shown inFIG. 23(B), as shown by the dotted line, a part having a smallersectional area than other sites of the groove 112 can be formed on theouter flat surface 113.

The groove 112 may be formed so as to be gradually decreased in size inthe direction from inside to outside as described above, and the part(terminal) of the groove 112 that had reached the outer periphery of thefirst processing member 101 may have the minimum sectional area (notshown). However, the groove 112 preferably does not penetrate to theouter periphery of the first processing member 101 as shown in FIG. 19and FIG. 21 to FIG. 23, in order to effectively generate dynamicalpressure.

Now, the embodiments shown in FIG. 18 to FIG. 23 are summarized.

This fluid processing apparatus is a processing apparatus wherein arotating member having a flat processing surface and a fixed memberhaving the same flat processing surface are opposite to each other so asto be concentric with each other, and while the rotating member isrotated, a raw material to be processed is fed through an opening of thefixed member and subjected to processing between the opposite flatprocessing surfaces of both members, wherein the rotating member isprovided with a pressurizing mechanism by which pressure is generated tomaintain clearance without mechanically regulating clearance and enables1 μm to 6 μm microscopic clearance not attainable by mechanicalregulation of clearance, thereby significantly improving an ability touniformize the mixing (reaction) and in some cases, an ability topulverize the formed particles.

That is, this fluid processing apparatus have a rotating member and afixed member each having a flat processing surface in the outerperiphery thereof and has a sealing mechanism in a plane on the flatprocessing surface, thereby providing a high speed rotation processingapparatus generating hydrostatic force, hydrodynamic force, oraerostatic-aerodynamic force. The force generates a minute space betweenthe sealed surfaces, and provides a fluid processing apparatus with afunction of non-contact and mechanically safe and high-leveluniformization of mixing (reaction). One factor for forming this minutespace is due to the rotation speed of the rotating member, and the otherfactor is due to a pressure difference between the introduction side anddischarge side of a processed material (fluid). When a pressureimparting mechanism is arranged in the introduction side, when thepressure imparting mechanism is not arranged in the introduction side,that is, when the processed material (fluid) is introduced atatmospheric pressure, there is no pressure difference, and thus thesealed surfaces should be separated by only the rotation speed of therotating member. This is known as hydrodynamic or aerodynamic force.

FIG. 18(A) shows the apparatus wherein a decompression pump Q isconnected to the discharge part of the mixing apparatus G, but asdescribed above, the mixing apparatus G may be arranged in adecompression tank T without arranging the housing 106 and thedecomposition pump Q, as shown in FIG. 24(A).

In this case, the tank T is decompressed in a vacuum or in an almostvacuum, whereby the processed product formed in the mixing apparatus Gis sprayed in a mist form in the tank T, and the processed materialcolliding with, and running down along, the inner wall of the tank T canbe recovered, or a gas (vapor) separated from the processed material andfilled in an upper part of the tank T, unlike the processed materialrunning down along the wall, can be recovered to obtain the objectiveproduct after processing.

When the decompression pump Q is used, as shown in FIG. 24(B), anairtight tank T is connected via the decompression pump Q to the mixingapparatus G, whereby the processed material after processing can beformed into mist to separate and extract the objective product.

As shown in FIG. 24(C), the decompression pump Q is connected directlyto the tank T, and the decompression pump Q and a discharge part forfluid R, different from the decompression pump Q, are connected to thetank T, whereby the objective product can be separated. In this case, agasified portion is sucked by the decompression pump Q, while the fluidR (liquid portion) is discharged from the discharge part separately fromthe gasified portion.

In the embodiments described above, the first and second processedfluids are introduced via the second holders 21 and 121 and the secondrings 20 and 102 respectively and mixed (reacted) with each other.

Now, other embodiments with respect to introduction of fluids to beprocessed into the apparatus are described.

As shown in FIG. 1(B), the processing apparatus shown in FIG. 1(A) isprovided with a third introduction part d3 to introduce a third fluid tobe processed into the space between the processing surfaces 1 and 2, andthe third fluid is mixed (reacted) with the first processed fluid aswell as the second processed fluid.

By the third introduction part d3, the third fluid to be mixed with thefirst processed fluid is fed to the space between the processingsurfaces 1 and 2. In this embodiment, the third introduction part d3 isa fluid flow path arranged in the second ring 20 and is open at one endto the second processing surface 2 and has a third fluid feed part p3connected to the other end.

In the third fluid feed part p3, a compressor or another pump can beused.

The opening of the third introduction part d3 in the second processingsurface 2 is positioned outside, and more far from, the rotation centerof the first processing surface 1 than the opening of the secondintroduction part d2. That is, in the second processing surface 2, theopening of the third introduction part d3 is located downstream from theopening of the second introduction part d2. A gap is arranged betweenthe opening of the third introduction part d3 and the opening of thesecond introduction part d2 in the radial direction of the second ring20.

With respect to structures other than the third introduction part d3,the apparatus shown in FIG. 1(B) is similar to that in the embodiment asin FIG. 1(A). In FIG. 1(B) and further in FIG. 1(C), FIG. 1(D) and FIG.2 to FIG. 11 described later, the case 3 is omitted to simplify thedrawings. In FIG. 9(B), FIG. 9(C), FIG. 10, FIG. 11(A) and FIG. 11(B), apart of the case 3 is shown.

As shown in FIG. 1(C), the processing apparatus shown in FIG. 1(B) isprovided with a fourth introduction part d4 to introduce a fourth fluidto be processed into the space between the processing surfaces 1 and 2,and the fourth fluid is mixed (reacted) with the first processed fluidas well as the second and third processed fluids.

By the fourth introduction part d4, the fourth fluid to be mixed withthe first processed fluid is fed to the space between the processingsurfaces 1 and 2. In this embodiment, the fourth introduction part d4 isa fluid flow path arranged in the second ring 20, is open at one end tothe second processing surface 2, and has a fourth fluid feed part p4connected to the other end.

In the fourth fluid feed part p4, a compressor or another pump can beused.

The opening of the fourth introduction part d4 in the second processingsurface 2 is positioned outside, and more far from, the rotation centerof the first processing surface 1 than the opening of the thirdintroduction part d3. That is, in the second processing surface 2, theopening of the fourth introduction part d4 is located downstream fromthe opening of the third introduction part d3.

With respect to structures other than the fourth introduction part d4,the apparatus shown in FIG. 1(C) is similar to that in the embodiment asin FIG. 1(B).

Five or more introduction parts further including a fifth introductionpart, a sixth introduction part and the like can be arranged to mix(react) five or more fluids to be processed with one another.

As shown in FIG. 1(D), the first introduction part d1 arranged in thesecond holder 21 in the apparatus in FIG. 1(A) can, similarly in thesecond introduction part d2, be arranged in the second processingsurface 2 in place of the second holder 21. In this case, the opening ofthe first introduction part d1 is located at the upstream side from thesecond introduction part d2, that is, it is positioned nearer to therotation center than the second introduction part d2 in the secondprocessing surface 2.

In the apparatus shown in FIG. 1(D), the opening of the secondintroduction part d2 and the opening of the third introduction part d3both are arranged in the second processing surface 2 of the second ring20. However, arrangement of the opening of the introduction part is notlimited to such arrangement relative to the processing surface.Particularly as shown in FIG. 2(A), the opening of the secondintroduction part d2 can be arranged in a position adjacent to thesecond processing surface 2 in the inner periphery of the second ring20. In the apparatus shown in FIG. 2(A), the opening of the thirdintroduction part d3 is arranged in the second processing surface 2similarly to the apparatus shown in FIG. 1(B), but the opening of thesecond introduction part d2 can be arranged inside the second processingsurface 2 and adjacent to the second processing surface 2, whereby thesecond processed fluid can be immediately introduced onto the processingsurfaces.

In this manner, the opening of the first introduction part d1 isarranged in the second holder 21, and the opening of the secondintroduction part d2 is arranged inside the second processing surface 2and adjacent to the second processing surface 2 (in this case,arrangement of the third introduction part d3 is not essential), so thatparticularly in reaction of a plurality of processed fluids, theprocessed fluid introduced from the first introduction part d1 and theprocessed fluid introduced from the second introduction part d2 areintroduced, without being reacted with each other, into the spacebetween the processing surfaces 1 and 2, and then both the fluids can bereacted first between the processing surfaces 1 and 2. Accordingly, thestructure described above is suitable for obtaining a particularlyreactive processed fluid.

The term “adjacent” is not limited to the arrangement where the openingof the second introduction part d2 is contacted with the inner side ofthe second ring 20 as shown in FIG. 2(A). The distance between thesecond ring 20 and the opening of the second introduction part d2 may besuch a degree that a plurality of processed fluids are not completelymixed (reacted) with one another prior to introduction into the spacebetween the processing surfaces 1 and 2. For example, the opening of thesecond introduction part d2 may be arranged in a position near thesecond ring 20 of the second holder 21. Alternatively, the opening ofthe second introduction part d2 may be arranged on the side of the firstring 10 or the first holder 11.

In the apparatus shown in FIG. 1(B), a gap is arranged between theopening of the third introduction part d3 and the opening of the secondintroduction part d2 in the radial direction of the second ring 20, butas shown in FIG. 2(B), the second and third processed fluids can beintroduced into the space between the processing surfaces 1 and 2,without providing such gap, thereby immediately joining both the fluidstogether. The apparatus shown in FIG. 2(B) can be selected depending onthe object of processing.

In the apparatus shown in FIG. 1(D), a gap is also arranged between theopening of the first introduction part d1 and the opening of the secondintroduction part d2 in the radial direction of the second ring 20, butthe first and second processed fluids can be introduced into the spacebetween the processing surfaces 1 and 2, without providing such gap,thereby immediately joining both the fluids together (not shown). Sucharrangement of the opening can be selected depending on the object ofprocessing.

In the embodiment shown in FIG. 1(B) and FIG. 1(C), the opening of thethird introduction part d3 is arranged in the second processing surface2 downstream from the opening of the second introduction part d2, inother words, outside the opening of the second introduction part d2 inthe radial direction of the second ring 20. Alternatively, as shown inFIG. 2(C) and FIG. 3(A), the opening of the third introduction part d3and the opening of the second introduction part d2 can be arranged inthe second processing surface 2 in positions different in acircumferential direction r0 of the second ring 20. In FIG. 3, numeralm1 is the opening (first opening) of the first introduction part d1,numeral m2 is the opening (second opening) of the second introductionpart d2, numeral m3 is the opening (third opening) of the thirdintroduction part d3, and numeral r1 is the radical direction of thering.

When the first introduction part d1 is arranged in the second ring 20,as shown in FIG. 2(D), the opening of the first introduction part d1 andthe opening of the second introduction part d2 can be arranged in thesecond processing surface 2 in positions different in thecircumferential direction of the second ring 20.

In the apparatus shown in FIG. 3(A), the openings of two introductionparts are arranged in the second processing surface 2 of the second ring20 in positions different in the circumferential direction r0, but asshown in FIG. 3(B), the openings of three introduction parts can bearranged in positions different in the circumferential direction r0 ofthe ring, or as shown in FIG. 3(C), the openings of four introductionparts can be arranged in positions different in the circumferentialdirection r0 of the ring. In FIG. 3(B) and FIG. 3(C), numeral m4 is theopening of the fourth introduction part, and in FIG. 3(C), numeral m5 isthe opening of the fifth introduction part. Five or more openings ofintroduction parts may be arranged in positions different in thecircumferential direction r0 of the ring (not shown).

In the apparatuses shown in above, the second to fifth introductionparts can introduce different fluids, that is, the second, third, fourthand fifth fluids. On the other hand, the second to fifth openings m2 tom5 can introduce the same fluid, that is, the second fluid into thespace between the processing surfaces. In this case, the second to fifthintroduction parts are connected to the inside of the ring and can beconnected to one fluid feed part, that is, the second fluid feed part p2(not shown).

A plurality of openings of introduction parts arranged in positionsdifferent in the circumferential direction r0 of the ring can becombined with a plurality of openings of introduction parts arranged inpositions different in the radial direction r1 of the ring.

For example, as shown in FIG. 3(D), the openings m2 to m9 of eightintroduction parts are arranged in the second processing surface 2,wherein four openings m2 to m5 of them are arranged in positionsdifferent in the circumferential direction r0 of the ring and identicalin the radial direction r1 of the ring, and the other four openings m6to m9 are arranged in positions different in the circumferentialdirection r0 of the ring and identical in the radial direction r1 of thering. Then, the other openings m6 to m9 are arranged outside the radialdirection r of the four openings m2 to m5. The outside openings andinside openings may be arranged in positions identical in thecircumferential direction r0 of the ring, but in consideration ofrotation of the ring, may be arranged in positions different in thecircumferential direction r0 of the ring as shown in FIG. 3(D). In thiscase too, the openings are not limited to the arrangement and numbershown in FIG. 3(D).

For example, as shown in FIG. 3(E), the outside opening in the radialdirection can be arranged in the apex of a polygon, that is, in the apexof a rectangle in this case, and the inside opening in the radialdirection can be positioned on one side of the rectangle. As a matter ofcourse, other arrangements can also be used.

When the openings other than the first opening m1 feed the secondprocessed fluid into the space between the processing surfaces, each ofthe openings may be arranged as continuous openings in thecircumferential direction r0 as shown in FIG. 3(F), instead of beingarranged discretely in the circumferential direction r0 of theprocessing surface.

As shown in FIG. 4(A), depending on the object of processing, the secondintroduction part d2 arranged in the second ring 20 in the apparatusshown in FIG. 1(A) can be, similar to the first introduction part d1,arranged in the central portion 22 of the second holder 21. In thiscase, the opening of the second introduction part d2 is positioned witha gap outside the opening of the first introduction part d1 positionedin the center of the second ring 20. As shown in FIG. 4(B), in theapparatus shown in FIG. 4(A), the third introduction part d3 can bearranged in the second ring 20. As shown in FIG. 4(C), in the apparatusshown in FIG. 4(A), the second and third processed fluids can beintroduced into the space inside the second ring 20 without arranging agap between the opening of the first introduction part d1 and theopening of the second introduction part d2, so that both the fluids canimmediately join together. As shown in FIG. 4(D), depending on theobject of processing, in the apparatus shown in FIG. 4(A), the thirdintroduction part d3 can be, similar to the second introduction part d2,arranged in the second holder 21. Four or more introduction parts may bearranged in the second holder 21 (not shown).

As shown in FIG. 5(A), depending on the object of processing, in theapparatus shown in FIG. 4(D), the fourth introduction part d4 can bearranged in the second ring 20, so that the fourth processed fluid maybe introduced into the space between the processing surfaces 1 and 2.

As shown in FIG. 5(B), in the apparatus shown in FIG. 1(A), the secondintroduction part d2 can be arranged in the first ring 10, and theopening of the second introduction part d2 can be arranged in the firstprocessing surface 1.

As shown in FIG. 5(C), in the apparatus shown in FIG. 5(B), the thirdintroduction part d3 can be arranged in the first ring 10, and theopening of the third introduction part d3 and the opening of the secondintroduction part d2 can be arranged in the first processing surface 1in positions different in the circumferential direction of the firstring 10.

As shown in FIG. 5(D), in the apparatus shown in FIG. 5(B), the firstintroduction part d1 can be arranged in the second ring 20 instead ofarranging the first introduction part d1 in the second holder 21, andthe opening of the first introduction part d1 can be arranged in thesecond processing surface 2. In this case, the openings of the first andsecond introduction parts d1 and d2 are arranged in positions identicalin the radial direction of the ring.

As shown in FIG. 6(A), in the apparatus shown in FIG. 1(A), the thirdintroduction part d3 can be arranged in the first ring 10, and theopening of the third introduction part d3 can be arranged in the firstprocessing surface 1. In this case, both the openings of the second andthird introduction parts d2 and d3 are arranged in positions identicalin the radial direction of the ring. However, both the openings may bearranged in positions different in the radial direction of the ring.

In the apparatus shown in FIG. 5(C), both the openings of the second andthird introduction parts d2 and d3 are arranged in positions identicalin the radial direction of the first ring 10 and simultaneously arrangedin positions different in the circumferential direction (that is,rotation direction) of the first ring 10, however in this apparatus, asshown in FIG. 6(B), both the openings of the second and thirdintroduction parts d2 and d3 can be arranged in positions identical inthe circumferential direction of the first ring 10 and simultaneouslyarranged in positions different in the radical direction of the firstring 10. In this case, as shown in FIG. 6(B), a gap can be arrangedbetween both the openings of the second and third introduction parts d2and d3 in the radial direction of the first ring 10, or withoutarranging the gap, the second and third processed fluids may immediatelyjoin together (not shown).

As shown in FIG. 6(C), the first introduction part d1 together with thesecond introduction part d2 can be arranged in the first ring 10 insteadof arranging the first introduction part d1 in the second holder 21. Inthis case, in the first processing surface 1, the opening of the firstintroduction part d1 is arranged upstream (inside the radial directionof the first ring 11) from the opening of the second introduction partd2. A gap is arranged between the opening of the first introduction partd1 and the opening of the second introduction part d2 in the radialdirection of the first ring 11. Alternatively, such gap may not bearranged (not shown).

As shown in FIG. 6(D), both the openings of the first introduction partd1 and the second introduction part d2 can be arranged in positionsdifferent in the circumferential direction of the first ring 10 in thefirst processing surface 1 in the apparatus shown in FIG. 6(C).

In the embodiment shown in FIG. 6(C) and FIG. 6(D), three or moreintroduction parts may be arranged in the first ring 10, and in thesecond processing surface 2, so the respective openings may be arrangedin positions different in the circumferential direction or in positionsdifferent in the radial direction of the ring (not shown). For example,the arrangement of openings in the second processing surface 2, shown inFIG. 3(B) to FIG. 3(F), can also be used in the first processing surface1.

As shown in FIG. 7(A), in the apparatus shown in FIG. 1(A), the secondintroduction part d2 can be arranged in the first holder 11 instead ofarranging the part d2 in the second ring 20. In this case, the openingof the second introduction part d2 is arranged preferably in the centerof the central shaft of rotation of the first ring 10, in the sitesurrounded with the first ring 10 on the upper surface of the firstholder 11.

As shown in FIG. 7(B), in the embodiment shown in FIG. 7(A), the thirdintroduction part d3 can be arranged in the second ring 20, and theopening of the third introduction part d3 can be arranged in the secondprocessing surface 2.

As shown in FIG. 7(C), the first introduction part d1 can be arranged inthe first holder 11 instead of arranging the part d1 in the secondholder 21. In this case, the opening of the first introduction part d1is arranged preferably in the central shaft of rotation of the firstring 10, in the site surrounded with the first ring 10 on the uppersurface of the first holder 11. In this case, as shown in the figure,the second introduction part d2 can be arranged in the first ring 10,and its opening can be arranged in the first processing surface 1. Inthis case, the second introduction part d2 can be arranged in the secondring 20, and its opening can be arranged in the second processingsurface 2 (not shown).

As shown in FIG. 7(D), the second introduction part d2 shown in FIG.7(C) together with the first introduction part d1 can be arranged in thefirst holder 11. In this case, the opening of the second introductionpart d2 is arranged in the site surrounded with the first ring 10 on theupper surface of the first holder 11. In this case, the secondintroduction part d2 arranged in the second ring 20 may serve as thethird introduction part d3 in FIG. 7(C).

In the embodiments shown in FIG. 1 to FIG. 7, the first holder 11 andthe first ring 10 are rotated relative to the second holder 21 and thesecond ring 20, respectively. As shown in FIG. 8(A), in the apparatusshown in FIG. 1(A), the second holder 2 may be provided with a rotaryshaft 51 rotating with the turning force from the rotation drive member,to rotate the second holder 21 in a direction opposite to the firstholder 11. The rotation drive member in the rotary shaft 51 may bearranged separately from the one for rotating the rotary shaft 50 of thefirst holder 11 or may receive power from the drive part for rotatingthe rotary shaft 50 of the first holder 11 by a power transmission meanssuch as a gear. In this case, the second holder 2 is formed separatelyfrom the case, and shall, like the first holder 11, be rotatablyaccepted in the case.

As shown in FIG. 8(B), in the apparatus shown in FIG. 8(A), the secondintroduction part d2 can be, similarly in the apparatus in FIG. 7(B),arranged in the first holder 11 in place of the second ring 20.

In the apparatus shown in FIG. 8(B), the second introduction part d2 canbe arranged in the second holder 21 in place of the first holder 11 (notshown). In this case, the second introduction part d2 is the same as onein the apparatus in FIG. 4(A). As shown in FIG. 8(C), in the apparatusshown in FIG. 8(B), the third introduction part d3 can be arranged inthe second ring 20, and the opening of the third introduction part d3can be arranged in the second processing surface 2.

As shown in FIG. 8(D), the second holder 21 only can be rotated withoutrotating the first holder 11. Even in the apparatuses shown in FIG. 1(B)to FIG. 7, the second holder 21 together with the first holder 11, orthe second holder 21 alone, can be rotated (not shown).

As shown in FIG. 9(A), the second processing member 20 is a ring, whilethe first processing member 10 is not a ring and can be a rotatingmember provided directly with a rotary shaft 50 similar to that of thefirst holder 11 in other embodiments. In this case, the upper surface ofthe first processing member 10 serves as the first processing surface 1,and the processing surface is an evenly flat surface which is notcircular (that is, hollow-free). In the apparatus shown in FIG. 9(A),similarly in the apparatus in FIG. 1(A), the second introduction part d2is arranged in the second ring 20, and its opening is arranged in thesecond processing surface 2.

As shown in FIG. 9(B), in the apparatus shown in FIG. 9(A), the secondholder 21 is independent of the case 3, and a surface-approachingpressure imparting mechanism 4 such as an elastic body for approachingto and separating from the first processing member 10 provided with thesecond ring 20 can be provided between the case 3 and the second holder21. In this case, as shown in FIG. 9(C), the second processing member 20is not a ring, but is a member corresponding to the second holder 21,and the lower surface of the member can serve as the second processingsurface 2. As shown in FIG. 10(A), in the apparatus shown in FIG. 9(C),the first processing member 10 is not a ring either, and in otherembodiments similarly in the apparatus shown in FIG. 9(A) and FIG. 9(B),the site corresponding to the first holder 11 can serve as the firstprocessing member 10, and its upper surface can serve as the firstprocessing surface 1.

In the embodiments described above, at least the first fluid is suppliedfrom the first processing member 10 and the second processing member 20,that is, from the central part of the first ring 10 and the second ring20, and after processing (mixing (reaction)) of the other fluids, theprocessed fluid is discharged to the outside in the radial direction.

Alternatively, as shown in FIG. 10(B), the first fluid can be suppliedin the direction from the outside to the inside of the first ring 10 andsecond ring 20. In this case, the outside of the first holder 11 and thesecond holder 21 is sealed with the case 3, the first introduction partd1 is arranged directly in the case 3, and the opening of theintroduction part is arranged in a site inside the case andcorresponding to the abutting position of the rings 10 and 20, as shownin the figure. In the apparatus in FIG. 1(A), a discharge part 36 isarranged in the position in which the first introduction part d1 isarranged, that is, in the central position of the ring 1 of the firstholder 11. The opening of the second introduction part d2 is arranged inthe opposite side of the opening of the case behind the central shaft ofrotation of the holder. However, the opening of the second introductionpart d may be, similar to the opening of the first introduction part d1,arranged in a site inside the case and corresponding to the abuttingposition of the rings 10 and 20. As described above, the embodiment isnot limited to the one where the opening of the second introduction partd is formed to the opposite side of the opening of the firstintroduction part d1.

In this case, the outside of the diameter of both the rings 10 and 20 ison the upstream side, and the inside of both the rings 10 and 20 is onthe downstream side.

As such, as shown in FIG. 16(E), when the processed fluid moves fromoutside to inside, the first processing surface 1 of the firstprocessing member 10 may also be provided with groove-like depressions13 . . . 13 extending in the direction from the outside to the center ofthe first processing member 10. When the groove-like depressions 13 . .. 13 are formed, the balance ratio K described above is preferably setas 100% or more of unbalance type. As a result, dynamical pressure isgenerated in the groove-like depressions 13 . . . 13 upon rotating, thefirst and second processing surfaces 1 and 2 can rotate in a surelynon-contact state, so that the risk of abrasion and the like due tocontact can be eliminated. In the embodiment shown in FIG. 16(E), theseparating force due to the pressure of the processed fluid is generatedin an inner end 13 a of the depressions 13.

As shown in FIG. 10(C), in the apparatus shown in FIG. 10(B), the secondintroduction part d2, which is arranged in the side of the case 3, canbe arranged in the first ring 11 in space of the mentioned position, andits opening can be arranged in the first processing surface 1. In thiscase, as shown in FIG. 10(D), the first processing member 10 is notformed as a ring. Similarly in the apparatuses shown in FIG. 9(A), FIG.9(B) and FIG. 10(A), in other embodiments, the site corresponding to thefirst holder 11 is the first processing member 10, its upper surfacebeing the first processing surface 1, the second introduction part d2being arranged in the first processing member 10, and its opening may bearranged in the first processing surface 1.

As shown in FIG. 11(A), in the apparatus shown in FIG. 10(D), the secondprocessing member 20 is not formed as a ring, and in other embodiments,the member corresponding to the second holder 21 serves as the secondprocessing member 20, and its lower surface serves as the secondprocessing surface 2. Then, the second processing member 20 is a memberindependent of the case 3, and the same surface-approaching pressureimparting mechanism 4 as one in the apparatuses shown in FIG. 9(B), FIG.9(C) and FIG. 10(A) can be arranged between the case 3 and the secondprocessing member 20.

As shown in FIG. 11(B), the second introduction part d2 in the apparatusshown in FIG. 11(A) serves as the third introduction part d3, andseparately the second introduction part d2 can be arranged. In thiscase, the opening of the second introduction part d2 is arrangeddownstream from the opening of the third introduction part d3 in thesecond processing surface 2.

In the apparatuses shown in FIG. 4 and the apparatuses shown in FIG.5(A), FIG. 7(A), FIG. 7(B), FIG. 7(D), FIG. 8(B) and FIG. 8(C), otherprocessed fluids flow into the first processed fluid before reaching theprocessing surfaces 1 and 2, and these apparatuses are not suitable forthe fluid which is rapidly crystallized or separated. However, theseapparatuses can be used for the fluid having a low reaction speed.

The fluid processing apparatus suitable for carrying out the methodaccording to the present invention is summarized as follows.

As described above, the fluid processing apparatus comprises a fluidpressure imparting mechanism that imparts predetermined pressure to aprocessed fluid, at least two processing members, that is, a firstprocessing member 10 arranged in a sealed fluid flow path through whicha processed fluid at the predetermined pressure flows and a secondprocessing member 20 capable of approaching to and separating from thefirst processing member 10, at least two processing surfaces of a firstprocessing surface 1 and a second processing surface 2 arranged in aposition in which they are faced with each other in the processingmembers 10 and 20, and a rotation drive mechanism that relativelyrotates the first processing member 10 and the second processing member20, wherein at least two processed fluids are mixed (and reacted whenthe mixing is accompanied by reaction) between the processing surfaces 1and 2. Of the first processing member 10 and the second processingmember 20, at least the second processing member 20 has apressure-receiving surface, at least a part of the pressure-receivingsurface is comprised of the second processing surface 2, and thepressure-receiving surface receives pressure applied by the fluidpressure imparting mechanism to at least one of the fluids to generate aforce to move in the direction of separating the second processingsurface 2 from the first processing surface 1. In this apparatus, theprocessed fluid that has received said pressure passes through the spacebetween the first processing surface 1 and the second processing surface2 capable of approaching to and separating from each other, therebygenerating a desired mixing (reaction) between the processed fluids withthe processed fluids being passed between the processing surfaces 1 and2 and forming a fluid film of predetermined thickness.

In this fluid processing apparatus, at least one of the first processingsurface 1 and the second processing surface 2 is preferably providedwith a buffer mechanism for regulation of micro-vibration and alignment.

In this processing apparatus, one of or both the first processingsurface 1 and the second processing surface 2 is preferably providedwith a displacement regulating mechanism capable of regulating thedisplacement in the axial direction caused by abrasion or the likethereby maintaining the thickness of a fluid film between the processingsurfaces 1 and 2.

In this fluid processing apparatus, a pressure device such as acompressor for applying predetermined feeding pressure to a fluid can beused as the fluid pressure imparting mechanism.

As the pressure device, a device capable of regulating an increase anddecrease in feeding pressure is used. This is because the pressuredevice should be able to keep established pressure constant and shouldbe able to regulate an increase and decrease in feeding pressure as aparameter to regulate the distance between the processing surfaces.

The fluid processing apparatus can be provided with a separationpreventing part for defining the maximum distance between the firstprocessing surface 1 and the second processing surface 2 and preventingthe processing surfaces 1 and 2 from separating from each other by themaximum distance or more.

The fluid processing apparatus can be provided with an approachpreventing part for defining the minimum distance between the firstprocessing surface 1 and the second processing surface 2 and preventingthe processing surfaces 1 and 2 from approaching to each other by theminimum distance or less.

The fluid processing apparatus can be one wherein both the firstprocessing surface 1 and the second processing surface 2 are rotated inopposite directions.

The fluid processing apparatus can be provided with atemperature-regulating jacket for regulating the temperature of eitheror both of the first processing surface 1 and the second processingsurface 2.

The fluid processing apparatus is preferably one wherein at least a partof either or both of the first processing surface 1 and the secondprocessing surface 2 is mirror-polished.

The fluid processing apparatus can be one wherein one of or both thefirst processing surface 1 and the second processing surface 2 isprovided with depressions.

The fluid processing apparatus preferably includes, as a means forfeeding one processed fluid to be mixed (reacted) with another processedfluid, a separate introduction path independent of a path for anotherprocessed fluid, at least one of the first processing surface and thesecond processing surface is provided with an opening leading to theseparate introduction path, and another processed fluid sent through theseparate introduction path is introduced into the processed fluid.

The fluid processing apparatus for carrying out the present inventioncomprises a fluid pressure imparting mechanism that impartspredetermined pressure to a fluid, at least two processing surfaces of afirst processing surface 1 and a second processing surface 2 capable ofapproaching to and separating from each other which are connected to asealed fluid flow path through which the processed fluid at thepredetermined pressure is passed, a surface-approaching pressureimparting mechanism that imparts surface-approaching pressure to thespace between the processing surfaces 1 and 2, and a rotation drivemechanism that relatively rotates the first processing surface 1 and thesecond processing surface 2, whereby at least two processed fluids aremixed (reacted) between the processing surfaces 1 and 2, at least oneprocessed fluid pressurized with the fluid pressure imparting mechanismis passed through the space between the first processing surface 1 andthe second processing surface 2 rotating to each other and supplied withsurface-approaching pressure, and another processed fluid is passed, sothat the processed fluid pressurized with the fluid pressure impartingmechanism, while being passed between the processing surfaces andforming a fluid film of predetermined thickness, is mixed with anotherprocessed fluid, whereby a desired mixing (reaction) is caused betweenthe processed fluids.

The surface-approaching pressure imparting mechanism can constitute abuffer mechanism of regulating micro-vibration and alignment and adisplacement regulation mechanism in the apparatus described above.

The fluid processing apparatus for carrying out the present inventioncomprises a first introduction part that introduces, into the apparatus,at least one of two processed fluids to be mixed (reacted), a fluidpressure imparting mechanism p that is connected to the firstintroduction part and imparts pressure to the processed fluid, a secondintroduction part that introduces at least the other fluid of the twoprocessed fluids to be mixed (reacted), at least two processing members,that is, a first processing member 10 arranged in a sealed fluid flowpath through which the other processed fluid is passed and a secondprocessing member 20 capable of relatively approaching to and separatingfrom the first processing member 10, at least two processing surfaces,that is, a first processing surface 1 and a second processing surface 2arranged so as to be opposite to each other in the processing members 10and 20, a holder 21 that accepts the second processing member 20 so asto expose the second processing surface 2, a rotation drive mechanismthat relatively rotates the first processing member 10 and the secondprocessing member 20, and a surface-approaching pressure impartingmechanism 4 that presses the second processing member 20 against thefirst processing surface 1 such that the second processing surface 2 iscontacted against or made close to the first processing surface 1,wherein the processed fluids are mixed (reacted) between the processingsurfaces 1 and 2, the holder 21 is provided with an opening of the firstintroduction part and is not movable so as to influence the spacebetween the processing surfaces 1 and 2, at least one of the firstprocessing member 10 and the second introduction part 20 is providedwith an opening of the second introduction part, the second processingmember 20 is circular, the second processing surface 2 slides along theholder 21 and approaches to and separates from the first processingsurface 1, the second processing member 20 includes a pressure-receivingsurface, the pressure-receiving surface receives pressure applied fromthe fluid pressure imparting mechanism p to the processed fluid togenerate a force to move in the direction of separating the secondprocessing surface 2 from the first processing surface 1, at least apart of the pressure-receiving surface is comprised of the secondprocessing surface 2, one of the processed fluids to which pressure wasapplied is passed through the space between the first processing surface1 and the second processing surface 2 rotating to each other and capableof approaching to and separating from each other, and the otherprocessed fluid is supplied to the space between the processing surfaces1 and 2, whereby both the processed fluids form a fluid film ofpredetermined thickness and pass through the space between both theprocessing surfaces 1 and 2, the passing processed fluid are mixedthereby promoting a desired mixing (reaction) between the processedfluids, and the minimum distance for generating the fluid film ofpredetermined thickness is kept between the processing surfaces 1 and 2by the balance between the surface-approaching pressure by thesurface-approaching pressure imparting mechanism 4 and the force ofseparating the processing surfaces 1 and 2 from each other by the fluidpressure imparted by the fluid pressure imparting mechanism p.

In this processing apparatus, the second introduction part can be,similarly being connected to the first introduction part, arranged to beconnected to a separate fluid pressure imparting mechanism and to bepressurized. The processed fluid introduced from the second introductionpart is not pressurized by the separate fluid pressure impartingmechanism, but is sucked and supplied into the space between theprocessing surfaces 1 and 2 by negative pressure generated in the secondintroduction part by the fluid pressure of the processed fluidintroduced into the first introduction part. Alternatively, the otherprocessed fluid flows downward by its weight in the second introductionpart and can be supplied into the space between the processing surfaces1 and 2.

As described above, the apparatus is not limited to the one wherein theopening of the first introduction part as an inlet for feeding the otherprocessed fluid into the apparatus is arranged in the second holder, andthe opening of the first introduction part may be arranged in the firstholder. The opening of the first introduction part may be formed with atleast one of the processing surfaces. However, when the processed fluidto be previously introduced into the space between the processingsurfaces 1 and 2 should, depending on the reaction, be supplied from thefirst introduction part, the opening of the second introduction part asan inlet for feeding the other processed fluid into the apparatus shouldbe arranged downstream from the opening of the first introduction partin any of the processing surfaces.

As the fluid processing apparatus for carrying out the presentinvention, the following apparatus can be used.

This processing apparatus comprises a plurality of introduction partsthat separately introduce two or more processed fluids to be mixed(reacted), a fluid pressure imparting mechanism p that imparts pressureto at least one of the two or more processed fluids, at least twoprocessing members, that is, a first processing member 10 arranged in asealed fluid flow path through which the processed fluid is passed and asecond processing member 20 capable of approaching to and separatingfrom the first processing member 10, at least two processing surfaces 1and 2, that is, a first processing surface 1 and a second processingsurface 2 arranged in a position in which they are faced with each otherin the processing members 10 and 20, and a rotation drive mechanism thatrelatively rotates the first processing member 10 and the secondprocessing member 20, wherein the processed fluids are mixed (reacted)between the processing surfaces 1 and 2, at least the second processingmember 20 of the first processing member 10 and the second processingmember 20 includes a pressure-receiving surface, at least a part of thepressure-receiving surface is comprised of the second processing surface2, the pressure-receiving surface receives pressure applied by the fluidpressure imparting mechanism to the processed fluid to generate a forceto move in the direction of separating the second processing surface 2from the first processing surface 1, the second processing member 20includes an approach regulating surface 24 that is directed to theopposite side of the second processing surface 2, the approachregulating surface 24 receives predetermined pressure applied to theprocessed fluid to generate a force to move in the direction ofapproaching the second processing surface 2 to the first processingsurface 1, a force to move in the direction of separating the secondprocessing surface 2 from the first processing surface 1 as a resultantforce of total pressure received from the processed fluid is determinedby the area ratio of the projected area of the approach regulatingsurface 24 in the approaching and separating direction to the projectedarea of the pressure-receiving surface in the approaching and separatingdirection, the processed fluid to which pressure was applied is passedthrough the space between the first processing surface 1 and the secondprocessing surface 2 that rotate relative to each other and capable ofapproaching to and separating from each other, the other processed fluidto be mixed (reacted) with the processed fluid is mixed in the spacebetween the processing surfaces, and the mixed processed fluid forms afluid film of predetermined thickness and simultaneously passes throughthe space between the processing surfaces 1 and 2, thereby giving adesired product while passing through the space between the processingsurfaces.

The fluid processing method according to the present invention issummarized as follows. The fluid processing method comprises applyingpredetermined pressure to a first fluid, connecting at least twoprocessing surfaces, that is, a first processing surface 1 and a secondprocessing surface 2, which are capable of approaching to and separatingfrom each other, to a sealed fluid flow path through which the processedfluid that has received the predetermined pressure is passed, applying asurface-approaching pressure of approaching the first processing surface1 and the second processing surface 2 each other, rotating the firstprocessing surface 1 and the second processing surface 2 relative toeach other, and introducing the processed fluid into the space betweenthe processing surfaces 1 and 2, wherein the second processed fluid tobe mixed (reacted) with the processed fluid is introduced through aseparate flow path into the space between the processing surfaces 1 and2 thereby mixing (reacting) both the processed fluids, the predeterminedpressure applied to at least the first processed fluid functions as aseparating force for separating the processing surfaces 1 and 2 fromeach other, and the separating force and the surface-approachingpressure are balanced via the processed fluid between the processingsurfaces 1 and 2, whereby the distance between the processing surfaces 1and 2 is kept in a predetermined minute space, the processed fluid ispassed as a fluid film of predetermined thickness through the spacebetween the processing surfaces 1 and 2, and when both the processedfluids are uniformly mixed (reacted) with each other while passing andaccompanied by separation, a desired reaction product is crystallized orseparated.

Hereinafter, other embodiments of the present invention are described indetail. FIG. 25 is a schematic sectional view of a fluid processingapparatus wherein materials to be processed are processed betweenprocessing surfaces, at least one of which rotates to the other, andwhich are capable of approaching to and separating from each other. FIG.26(A) is a schematic plane view of the first processing surface in theapparatus shown in FIG. 25, and FIG. 26(B) is an enlarged view of animportant part of the processing surface in the apparatus shown in FIG.25. FIG. 27(A) is a sectional view of the second introduction path, andFIG. 27(B) is an enlarged view of an important part for explaining thesecond introduction path.

In FIG. 25, arrows U and S show upward and downward directionsrespectively. In FIG. 26(A) and FIG. 27(B), arrow R shows the directionof rotation. In FIG. 27(B), arrow C shows the direction of centrifugalforce (radial direction).

This apparatus uses at least two fluids, at least one of which containsat least one kind of material to be processed, and the fluids jointogether in the space between the processing surfaces arranged to beopposite to each other so as to be able to approach to and separate fromeach other, at least one of which rotates relative to the other, therebyforming a thin film fluid, and the materials to be processed areprocessed in the thin film fluid. The “process” includes not only a formin which a processed material is reacted, but also a form in which onlymixing or dispersion is conducted without accompanying reaction.

As shown in FIG. 25, this apparatus includes a first holder 11, a secondholder 21 arranged over the first holder 11, a fluid pressure impartingmechanism P and a surface-approaching pressure imparting mechanism. Thesurface-approaching pressure imparting mechanism is comprised of aspring 43 and an air introduction part 44.

The first holder 11 is provided with a first processing member 10 and arotary shaft 50. The first processing member 10 is a circular bodycalled a maintaining ring and provided with a mirror-polished firstprocessing surface 1. The rotary shaft 50 is fixed to the center of thefirst holder 11 with a fixing device 81 such as a bolt and is connectedat its rear end to a rotation drive device 82 (rotation drive mechanism)such as a motor, and the drive power of the rotation drive device 82 istransmitted to the first holder 1 thereby rotating the first holder 11.The first processing member 10 is integrated with the first holder 11and rotated.

A receiving part capable of receiving the first processing member 10 isarranged on the upper part of the first holder 11, wherein the firstprocessing member 10 has been fixed to the first holder 11 by insertionto the receiving part. The first processing member 10 has been fixedwith a rotation preventing pin 83 so as not to be rotated relative tothe first holder 11. However, a method such as fitting by burning may beused for fixing in place of the rotation-preventing pin 83 in order toprevent rotation.

The first processing surface 1 is exposed from the first holder 11 andfaced with the second holder 21. The material for the first processingsurface includes ceramics, sintered metal, abrasion-resistant steel,other hardened metals, and rigid materials subjected to lining, coatingor plating.

The second holder 21 is provided with a second processing member 20, afirst introduction part d1 for introducing a fluid from the inside ofthe processing member, a spring 43 as a surface-approaching pressureimparting mechanism, and an air introduction part 44.

The second processing member 20 is a circular member called acompression ring and includes a second processing surface 2 subjected tomirror polishing and a pressure-receiving surface 23 (referred tohereinafter as a separation regulating surface 23) which is locatedinside the second processing surface 2 and adjacent to the secondprocessing surface 2. As shown in the figure, the separation regulatingsurface 23 is an inclined surface. The method of the mirror polishing towhich the second processing surface 2 was subjected is the same as thatto the first processing surface 1. The material for the secondprocessing member 20 may be the same as one for the first processingmember 10. The separation regulating surface 23 is adjacent to the innerperiphery 25 of the circular second processing member 20.

A ring-accepting part 41 is formed in the bottom (lower part) of thesecond holder 21, and the second processing member 20 together with anO-ring is accepted in the ring-accepting part 41. The second processingmember 20 is accepted with a rotation preventive 84 so as not to berotated relative to the second holder 21. The second processing surface2 is exposed from the second holder 21. In this state, the secondprocessing surface 2 is faced with the first processing surface 1 of thefirst processing member 10.

The ring-accepting part 41 arranged in the second holder 21 is adepression for mainly accepting that side of the second ring 20 which isopposite to the processing surface 2 and is a groove formed in acircular form when viewed in a plane.

The ring-accepting part 41 is formed in a larger size than the secondring 20 and accepts the second ring 20 with sufficient clearance betweenitself and the second ring 20.

By this clearance, the second processing member 20 is accepted in thering-accepting part 41 such that it can be displaced not only in theaxial direction of the accepting part 41 but also in a directionperpendicular to the axial direction. The second processing member 20 isaccepted in the ring-accepting part 41 such that the central line (axialdirection) of the second processing member 20 can be displaced so as notto be parallel to the axial direction of the ring-accepting part 41.

The spring 43 is arranged as a processing member-biasing part in atleast the ring-accepting part 41 of the second holder 21. The spring 43biases the second processing member 20 toward the first processingmember 10. As another bias method, air pressure such as one in the airintroduction part 44 or another pressurization means for applying fluidpressure may be used to bias the second processing member 20 held by thesecond holder 21 in the direction of approaching the second processingmember 20 to the first processing member 10.

The surface-approaching pressure imparting mechanism such as the spring43 or the air introduction part 44 biases each position (each positionin the processing surface) in the circumferential direction of thesecond processing member 20 evenly toward the first processing member10.

The first introduction part d1 is arranged on the center of the secondholder 21, and the fluid which is pressure-fed from the firstintroduction part d1 to the outer periphery of the processing member isfirst introduced into the space surrounded with the second processingmember 20 held by the second holder 21, the first processing member 10,and the first holder 11 that holds the first processing member 10. Then,the feeding pressure (supply pressure) of the fluid by the fluidpressure imparting mechanism P is applied to the pressure-receivingsurface 23 arranged in the second processing member 20, in the directionof separating the second processing member 20 from the first processingmember 10 against the bias of the biasing part.

For simplifying the description of other components, only thepressure-receiving surface 23 is described, as shown in FIG. 29(A) andFIG. 29(B), properly speaking, together with the pressure-receivingsurface 23, a part 23X not provided with the pressure-receiving surface23, out of the projected area in the axial direction relative to thesecond processing member 20 in a grooved depression 13 described later,serves as a pressure-receiving surface and receives the feeding pressure(supply pressure) of the fluid by the fluid pressure imparting mechanismP.

The apparatus may not be provided with the pressure-receiving surface23. In this case, as shown in FIG. 26(A), the effect (micro-pump effect)of introduction of the processed fluid into the space between theprocessing surfaces formed by rotation of the first processing surface 1provided with the grooved depression 13 formed to function thesurface-approaching pressure imparting mechanism may be used. Themicro-pump effect is an effect by which the fluid in the depression 13advances with speed toward the end in the circumferential direction byrotation of the first processing surface 1 and then the fluid sent tothe end of the depression 13 further receives pressure in the directionof inner periphery of the depression 13 thereby finally receivingpressure in the direction of separating the processing surface andsimultaneously introducing the fluid into the space between theprocessing surfaces. Even if the first processing surface 1 is notrotated, the pressure applied to the fluid in the depression 13 arrangedin the first processing surface 1 finally acts on the second processingsurface 2 to be separated as a pressure-receiving surface.

For the depression 13 arranged on the processing surface, its total areain the horizontal direction relative to the processing surface, and thedepth, number, and shape of depressions, can be established depending onthe physical properties of a fluid containing materials to be processedand reaction products.

The pressure-receiving surface 23 and the depression 13 may be arrangedin the same apparatus.

The depression 13 is a depression having a depth of 1 μm to 50 μm,preferably 3 μm to 20 μm, which is arranged on the processing surface,the total area thereof in the horizontal direction is 5% to 50%,preferably 15% to 25%, based on the whole of the processing surface, thenumber of depressions is 3 to 50, preferably 8 to 24, and the depressionextends in a curved or spiral form on the processing surface or bends ata right angle, having depth changing continuously, so that fluids withhigh to low viscosity, even containing solids, can be introduced intothe space between the processing surfaces stably by the micro-pumpeffect. The depressions arranged on the processing surface may beconnected to one another or separated from one another in the side ofintroduction, that is, inside the processing surface.

As described above, the pressure-receiving surface 23 is inclined. Thisinclined surface (pressure-receiving surface 23) is formed such that thedistance in the axial direction between the upstream end in thedirection of flow of the processed fluid and the processing surface ofthe processing member provided with the depression 13 is longer than thedistance between the downstream end and the aforesaid processingsurface. The downstream end of this inclined surface in the direction offlow of the processed fluid is arranged preferably on the projected areain the axial direction of the depression 13.

Specifically, as shown in FIG. 28(A), a downstream end 60 of theinclined surface (pressure-receiving surface 23) is arranged on theprojected area in the axial direction of the depression 13. The angle θ1of the inclined surface to the second processing surface 2 is preferablyin the range of 0.1° to 85°, more preferably in the range of 10° to 55°,still more preferably in the range of 15° to 45°. The angle θ1 can varydepending on properties of the processed product before processing. Thedownstream end 60 of the inclined surface is arranged in the regionextending from the position apart downstream by 0.01 mm from an upstreamend 13-b to the position apart upstream by 0.5 mm from a downstream end13-c in the depression 13 arranged in the first processing surface 1.The downstream end 60 of the inclined surface is arranged morepreferably in the region extending from the position apart downstream by0.05 mm from the upstream end 13-b to the position apart upstream by 1.0mm from the downstream end 13-c. Like the angle of the inclined surface,the position of the downstream end 60 can vary depending on propertiesof a material to be processed. As shown in FIG. 28(B), the inclinedsurface (pressure-receiving surface 23) can be a curved surface. Thematerial to be processed can thereby be introduced more uniformly.

The depressions 13 may be connected to one another or separated from oneanother as described above. When the depressions 13 are separated, theupstream end at the innermost peripheral side of the first processingsurface 1 is 13-b, and the upstream end at the outermost peripheral sideof the first processing surface 1 is 13-c.

In the foregoing description, the depression 13 was formed on the firstprocessing surface 1 and the pressure-receiving surface 23 was formed onthe second processing surface 2. On the contrary, the depression 13 maybe formed on the second processing surface 2, and the pressure-receivingsurface 23 may be formed on the first processing surface 1.

Alternatively, the depression 13 is formed both on the first processingsurface 1 and the second processing surface 2, and the depression 13 andthe pressure-receiving surface 23 are alternately arranged in thecircumferential direction of each of the respective processing surfaces1 and 2, whereby the depression 13 formed on the first processingsurface 1 and the pressure-receiving surface 23 formed on the secondprocessing surface 2 are faced with each other and simultaneously thepressure-receiving surface 23 formed on the first processing surface 1and the depression 13 formed on the second processing surface 2 arefaced with each other.

A groove different from the depression 13 can be formed on theprocessing surface. Specifically, as shown in FIG. 16(F) and FIG. 16(G),a radially extending novel depression 14 instead of the depression 13can be formed outward in the radial direction (FIG. 16(F)) or inward inthe radial direction (FIG. 16(G)). This is advantageous for prolongationof retention time between the processing surfaces or for processing ahighly viscous fluid.

The groove different from the depression 13 is not particularly limitedwith respect to the shape, area, number of depressions, and depth. Thegroove can be formed depending on the object.

The second introduction part d2 independent of the fluid flow pathintroduced into the processing surface and provided with the opening d20leading to the space between the processing surfaces is formed on thesecond processing member 20.

Specifically, as shown in FIG. 27(A), the direction of introduction ofthe second introduction part d2 from the opening d20 of the secondprocessing surface 2 is inclined at a predetermined elevation angle (θ1)relative to the second processing surface 2. The elevation angle (θ1) isarranged at more than 0° and less than 90°, and when the reaction speedis high, the angle (θ1) is preferably arranged at 1° to 45°.

As shown in FIG. 27(B), the direction of introduction of the secondprocessing surface 2 from the opening d20 has directionality in a planealong the second processing surface 2. The direction of introduction ofthe second fluid is in the direction in which a component on theprocessing surface is made apart in the radial direction and in thedirection in which the component is forwarded in the rotation directionof the fluid between the rotating processing surfaces. In other words, apredetermined angle (θ2) exists facing the rotation direction R from areference line g in the outward direction and in the radial directionpassing through the opening d20.

The angle (θ2) is also arranged at more than 0° and less than 90° atwhich the fluid is discharged from the opening d20 in the shaded regionin FIG. 27(B). When the reaction speed is high, the angle (θ2) may besmall, and when the reaction speed is low, the angle (θ2) is preferablyarranged larger. This angle can vary depending on various conditionssuch as the type of fluid, the reaction speed, viscosity, and therotation speed of the processing surface.

The bore diameter of the opening d20 is preferably 0.2 μm to 3000 μm,more preferably 10 μm to 1000 μm. When the diameter of the opening d20does not substantially influence the flow of a fluid, the diameter ofthe second introduction part d2 may be established in this range.Depending on whether the fluid is intended to be transferred straight ordispersed, the shape of the opening d20 is preferably changed and can bechanged depending on various conditions such as the type of fluid,reaction speed, viscosity, and rotation speed of the processing surface.

The opening d20 in the separate flow path may be arranged at a positionnearer to the outer diameter than a position where the direction of flowupon introduction by the micro-pump effect from the depression arrangedin the first processing surface 1 is converted into the direction offlow of a spiral laminar flow formed between the processing surfaces.That is, in FIG. 26(B), the distance n from the outermost side in theradial direction of the processing surface of the depression 13 arrangedin the first processing surface 1 to the outside in the radial directionis preferably 0.5 mm or more. When a plurality of openings are arrangedfor the same fluid, the openings are arranged preferably concentrically.When a plurality of openings are arranged for different fluids, theopenings are arranged preferably concentrically in positions differentin radius. This is effective for the reactions such as cases (1) A+B→Cand (2) C+D→E should occur in due order, but other case, i.e., A+B+C→Fshould not occur, or for circumventing a problem that an intendedreaction does not occur, due to insufficient contact among the processedmaterials.

The processing members are dipped in a fluid, and a fluid obtained bymixing (reaction) between the processing surfaces can be directlyintroduced into a liquid outside the processing members or into a gasother than air.

Further, ultrasonic energy can be applied to the processed material justafter being discharged from the space between the processing surfaces orfrom the processing surface.

Then, the case where temperature regulating mechanisms J1 and J2 arearranged in at least one of the first processing member 10 and thesecond processing member 20 for generating a temperature differencebetween the first processing surface 1 and the second processing surface2 is described.

The temperature regulating mechanism is not particularly limited. Acooling part is arranged in the processing members 10 and 201 whencooling is intended. Specifically, a piping for passing ice water andvarious cooling media or a cooling element such as a Peltier devicecapable of electric or chemical cooling is attached to the processingmembers 10 and 20.

When heating is intended, a heating part is arranged in the processingmembers 10 and 20. Specifically, steam as a temperature regulatingmedium, a piping for passing various hot media, and a heating elementsuch as an electric heater capable of electric or chemical heating isattached to the processing members 10 and 20.

An accepting part for a new temperature regulating medium capable ofdirectly contacting with the processing members may be arranged in thering-accepting part. The temperature of the processing surfaces can beregulated by heat conduction of the processing members. Alternatively, acooling or heating element may be embedded in the processing members 10and 20 and electrified, or a path for passing a cooling medium may beembedded, and a temperature regulating medium (cooling medium) is passedthrough the path, whereby the temperature of the processing surfaces canbe regulated from the inside. By way of example, the temperatureregulating mechanisms J1 and J2 which are pipes (jackets) arrangedinside the processing members 10 and 20 are shown in FIG. 25.

By utilizing the temperature regulating mechanisms J1 and J2, thetemperature of one of the processing surfaces is made higher than thatof the other, to generate a temperature difference between theprocessing surfaces. For example, the first processing member 10 isheated to 60° C. by any of the methods, and the second processing member20 is set at 15° C. by any of the methods. In this case, the temperatureof the fluid introduced between the processing surfaces is changed from60° C. to 15° C. in the direction from the first processing surface 1 tothe second processing surface 2. That is, the fluid between theprocessing surfaces has a temperature gradient. The fluid between theprocessing surfaces initiates convection due to the temperaturegradient, and a flow in a direction perpendicular to the processingsurface is generated. “The flow in a direction perpendicular to theprocessing surface” refers to a flow in which components flowing in adirection perpendicular to at least the processing surface are containedin flowing components.

Even when the first processing surface 1 or the second processingsurface 2 rotates, the flow in a direction perpendicular to theprocessing surface is continued, and thus the flow in a directionperpendicular to the processing surface can be added to a spiral laminarflow between the processing surfaces caused by rotation of theprocessing surfaces. The temperature difference between the processingsurfaces is 1° C. to 400° C., preferably 5° C. to 100° C.

The rotary shaft 50 in this apparatus is not limited to a verticallyarranged shaft. For example, the rotation axis may be arranged at aslant. This is because the influence of gravity can be substantiallyeliminated by a thin film formed between the processing surfaces 1 and 2during processing. As shown in FIG. 25, the first introduction part d1coincides with the shaft center of the second ring 20 in the secondholder 21 and extends vertically. However, the first introduction partd1 is not limited to the one coinciding with the shaft center of thesecond ring 20, and as far as it can supply the first processing fluidto the space surrounded with the rings 10 and 20, the part d1 may bearranged at a position outside the shaft center in the central part 22of the second holder 21 and may extend obliquely as well as vertically.Regardless of the angle at which the part d1 is arranged, a flowperpendicular to the processing surface can be generated by thetemperature gradient between the processing surfaces.

When the temperature gradient of the fluid between the processingsurfaces is low, heat conduction merely occurs in the fluid, but whenthe temperature gradient exceeds a certain border value, a phenomenoncalled Benard convection is generated in the fluid. This phenomenon isgoverned by Rayleigh number Ra, a dimensionless number, defined by thefollowing equation:Ra=L ³ ·g·βΔT/(α·ν)wherein L is the distance between processing surfaces; g isgravitational acceleration; β is coefficient of volumetric thermalexpansion of fluid; ν is dynamic viscosity of fluid; α is heatdiffusivity of fluid; and ΔT is temperature difference betweenprocessing surfaces. The critical Rayleigh number at which Benardconvection is initiated to occur, although varying depending on theproperties of a boundary phase between the processing surface and theprocessed fluid, is regarded as about 1700. At a value higher than thisvalue, Benard convection occurs. Under the condition where the Rayleighnumber Ra is a large value of about 10¹⁰ or more, the fluid becomes aturbulent flow. That is, the temperature difference ΔT between theprocessing surfaces or the distance L between the processing surfaces inthis apparatus are regulated such that the Rayleigh number Ra becomes1700 or more, whereby a flow perpendicular to the processing surface canbe generated between the processing surfaces, and the mixing (reaction)procedures described above can be carried out.

However, the Benard convection hardly occurs when the distance betweenthe processing surfaces is about 1 μm to 10 μm. Strictly, when theRayleigh number is applied to a fluid between the processing surfaceshaving a distance of 10 μm or less therebetween to examine theconditions under which Benard convection is generated, the temperaturedifference should be several thousands of degrees or more in the case ofwater, which is practically difficult. Benard convection is one relatedto density difference in temperature gradient of a fluid, that is, togravity. When the distance between the processing surfaces is 10 μm orless, there is high possibility of minute gravity field, and in such aplace, buoyancy convection is suppressed. That is, it is the case wherethe distance between the processing surfaces is 10 μm or more thatBenard convection actually occurs.

When the distance between the processing surfaces is about 1 μm to 10μm, convection is generated not due to density difference but due tosurface tension difference of a fluid resulting from temperaturegradient. Such convection is Marangoni convection. This phenomenon isgoverned by Marangoni number, a dimensionless number, defined by thefollowing equation:Ma=σ·ΔT·L/(ρ·ν·α)wherein L is the distance between processing surfaces; ν is dynamicviscosity of fluid; α is heat diffusivity of fluid; ΔT is temperaturedifference between processing surfaces; ρ is density of fluid; and σ istemperature coefficient of surface tension (temperature gradient ofsurface tension). The critical Marangoni number at which Marangoniconvection is initiated to occur is about 80, and under the conditionswhere the Marangoni number is higher than this value, Marangoniconvection occurs. That is, the temperature difference ΔT between theprocessing surfaces or the distance L between the processing surfaces inthis apparatus is regulated such that the Marangoni number Ma becomes 80or more, whereby a flow perpendicular to the processing surface can begenerated between the processing surfaces even if the distancetherebetween is as small as 10 μm or less, and the mixing (reaction)procedures described above can be carried out.

For calculation of Rayleigh number, the following equations were used.

$\begin{matrix}{{{Ra} = {\frac{L^{3} \cdot \beta \cdot g}{\nu \cdot \alpha}\Delta\; T}}{{\Delta\; T} = \left( {T_{1} - T_{0}} \right)}{\alpha = \frac{k}{\rho \cdot C_{p}}}} & \left\lbrack {{Equation}\mspace{14mu} 1} \right\rbrack\end{matrix}$L is the distance (m) between processing surfaces; β is coefficient ofvolumetric thermal expansion (1/K); g is gravitational acceleration(m/s²); ν is dynamic viscosity (m²/s); α is heat diffusivity (m²/s); ΔTis temperature difference (K) between processing surfaces;ρ is density (kg/m³); Cp is isobaric specific heat (J/kg·K);k is heat conductivity (W/m·K);T₁ is temperature (K) at high temperature side in processing surface;and T₀ is temperature (K) at low temperature side in processing surface.

When the Rayleigh number at which Benard convection is initiated tooccur is the critical Rayleigh number Ra_(C), the temperature differenceΔT_(C1) is determined as follows:

$\begin{matrix}{{\Delta\; T_{C\; 1}} = \frac{{Ra}_{c} \cdot \nu \cdot \alpha}{L^{3} \cdot \beta \cdot g}} & \left\lbrack {{Equation}\mspace{14mu} 2} \right\rbrack\end{matrix}$

For calculation of Marangoni number, the following equations were used.

$\begin{matrix}{{{Ma} = {\frac{\sigma_{t} \cdot L}{\rho \cdot \nu \cdot \alpha}\Delta\; T}}{{\Delta\; T} = \left( {T_{1} - T_{0}} \right)}{\alpha = \frac{k}{\rho \cdot C_{p}}}} & \left\lbrack {{Equation}\mspace{14mu} 3} \right\rbrack\end{matrix}$L is the distance (m) between processing surfaces; ν is dynamicviscosity (m²/s); α is heat diffusivity (m²/s);ΔT is temperature difference (K) between processing surfaces;ρ is density (kg/m³); Cp is isobaric specific heat (J/kg·K);k is heat conductivity (W/m·K); σ_(t) is surface tension temperaturecoefficient (N/m·k);T₁ is temperature (K) at high temperature side in processing surface;and T₀ is temperature (K) at low temperature side in processing surface.

When the Marangoni number at which Marangoni convection is initiated tooccur is the critical Marangoni number Ma_(C), the temperaturedifference ΔT_(C2) is determined as follows:

$\begin{matrix}{{\Delta\; T_{C\; 2}} = \frac{{Ma}_{c} \cdot \rho \cdot \nu \cdot \alpha}{\sigma_{t} \cdot L}} & \left\lbrack {{Equation}\mspace{14mu} 4} \right\rbrack\end{matrix}$

The materials for the processing surface arranged to be opposite to eachother so as to be able to approach to and separate from each other, atleast one of which rotates relative to the other, are not particularlylimited, and the processing surfaces 1 and 2 can be prepared fromceramics, sintered metals, abrasion-resistant steels, other metalssubjected to hardening treatment, or rigid materials subjected tolining, coating or plating. In the present invention, the distancebetween the processing surfaces 1 and 2 arranged to be opposite to eachother so as to be able to approach to and separate from each other, atleast one of which rotates relative to the other, is 0.1 μm to 100 μm,particularly preferably 1 μm to 10 μm.

Hereinafter, the reaction of forming magnetic microparticles accordingto the present invention is described in more detail.

This reaction occurs by forced uniform mixing between the processingsurfaces 1 and 2 arranged to be opposite to each other so as to be ableto approach to and separate from each other, at least one of whichrotates relative to the other, in the apparatus shown in FIG. 1(A).

First, a fluid containing at least one kind of magnetic material isintroduced through one flow path, that is, the first introduction partd1 into the space between the processing surfaces 1 and 2 arranged to beopposite to each other so as to be able to approach to and separate fromeach other, at least one of which rotates relative to the other, therebyforming a first fluid film between the processing surfaces.

Then, a fluid containing at least one kind of a magneticmicroparticle-separating agent such as a reducing agent is introduceddirectly as a second fluid through another flow path, that is, thesecond introduction part d2 into the first fluid film produced betweenthe processing surfaces 1 and 2.

As described above, a thin film fluid is formed between the processingsurfaces 1 and 2, the distance of which is regulated by the pressurebalance between the supply pressure of the fluid and the pressureexerted between the rotating processing surfaces. Then, the first fluidand the second fluid are allowed to join together in this thin filmfluid and mixed, thereby separating magnetic microparticles to effectthe reaction of forming magnetic microparticles. From the reactionprocessing apparatus, a magnetic fluid containing magneticmicroparticles is removed.

To effect the reaction between the processing surfaces 1 and 2, thesecond fluid may be introduced through the first introduction part d1and the first fluid through the second introduction part d2, as opposedto the above description. That is, the expression “first” or “second”for each fluid has a meaning for merely discriminating an n^(th) fluidamong a plurality of fluids present, and third or more fluids can alsobe present.

The particle size, monodispersity, and crystallinity and degree ofcrystallization of the obtained magnetic microparticles can be regulatedby changing the number of revolutions of the processing surfaces 1 and2, the distance between the processing surfaces 1 and 2, the flow rateand temperature of the thin film fluid, and the concentration ofmaterials.

Even when a reverse micelle method is used as a method of synthesizing amagnetic body, that is, when a first reverse micellar solution obtainedby adding a dispersant and an aqueous solution of a magnetic material toan organic solvent, and a second reverse micellar solution containing atleast one kind of a magnetic microparticle-separating agent, are used asthe first and second fluids respectively, a magnetic fluid and magneticmicroparticles can be prepared.

The metal contained in the magnetic microparticles obtained by theproduction method of the present invention is not particularly limitedas long as the metal has magnetism in the form of an element orcompound. The metal contained is preferably at least one transitionelement selected from nickel, cobalt, iridium, iron, platinum, gold,silver, manganese, chromium, palladium, yttrium, and lanthanides(neodymium, samarium, gadolinium and terbium).

The magnetic microparticles may contain elements other than thosedescribed above. Examples of such elements include copper, zinc,magnesium, rhenium, bismuth and silicon.

The magnetic microparticles described above may have physical propertiesother than magnetism, for example physical properties of semiconductors.For example, there are magnetic semiconductor microparticles comprisingCdCr₂Se₄ and EuX (X represents a group VI element such as S, Se or thelike) having a Curie temperature lower than 150 K.

In addition, there are magnetic semiconductor microparticles comprisingmixed crystal semiconductors wherein 3d transition metals such as Mn aremixed as magnetic elements in group II-VI compound semiconductors, groupIII-V compound semiconductors, group IV compound semiconductors andgroup I-III-VI compound semiconductor. In this example, there is CdMnTeor CdHgMnTe as typical group II-VI DMS (dilute magnetic semiconductor).As typical group III-V DMS, there are InMnAs (50 K), GaMnAs (160 K), andInGaMnAs (130 K). The numbers shown in parentheses indicateferromagnetic transition temperatures, and each of the substances showsferromagnetism at low temperatures.

Other examples include magnetic microparticles comprising BeMnZnSe.

On the other hand, the magnetic microparticles may be those not havingthe physical properties mentioned above. For example, iron-copperalloys, iron-platinum alloys, nickel, nickel-iron alloys, cobalt,cobalt-iron alloys, manganese, manganese-iron alloys, titanium,titanium-iron alloys, vanadium, vanadium-copper alloys, and magnetite(Fe₃O₄) are magnetic bodies which do not have physical properties ofsemiconductors.

However, even if each material unit has its single physical property,the product has a plurality of physical properties derived from each ofthe materials, in the case a different kind of material from the aboveis added to microparticles comprising a single material, or plural kindsof microparticles comprising a single material are aggregated to formaggregates. In the present invention, therefore, a product containing atleast magnetic microparticles is regarded as a magnetic product as faras among plural physical properties of the product, its magnetism isutilized. For example, an aggregate exhibiting physical properties bothas a magnetic material and as a semiconductor is regarded as a magneticproduct as far as its physical properties as a magnetic material aremainly utilized.

The magnetic product includes, for example, a product utilizing itsfixed magnetic pole (a permanent magnet), a product utilizing aphenomenon of shifting its magnetic pole (a core of an electric magnet,an aggregating agent comprising a magnet-binding polymer, amagnetism-imparting agent, and the like), a product utilizing partialmagnetism shifting (magnetic recording media such as magnetic disk) anda product blocking a magnetic field (a magnetic wave-shielding materialand the like). The magnetic product is not limited to solid one and maybe a powdery product (toner for printer, and the like) and a liquidproduct (magnetic fluid).

As the method for producing these magnetic products, various methods canbe used. For example, the magnetic products can be produced bysolidifying and molding, in various shapes, a large number ofmicroparticles containing magnetic microparticles and other materials,by mixing, in a resin or the like, a large number of microparticlescontaining magnetic microparticles, or by allowing a large number ofmicroparticles containing magnetic microparticles to be adhered, by ameans such as coating, deposition or sputtering, to the surface of adisk or the like. Further, a magnetic product can be produced bydispersing, in a colloidal state, a large number of microparticlescontaining magnetic microparticles in a fluid.

In the present invention, when magnetic microparticles are obtained in athin film fluid formed between the processing surfaces arranged to beopposite to each other so as to be able to approach to and separate fromeach other, at least one of which rotates relative to the other, therebypreparing magnetic microparticles comprising a metal such as FeCu(iron-copper alloy) microparticles, then an aqueous solution having aniron salt such as ferrous chloride and a copper salt such as coppersulfate dissolved in an aqueous solvent is used as a first fluid, and anaqueous solution wherein a reducing agent serving as a magneticmicroparticle-separating agent such as hydrazine or dimethylaminoethanolis dissolved is used as a second fluid, whereby FeCu microparticles canbe prepared. The aqueous solvent is not particularly limited, andpurified water such as ion-exchange water and pure water can be used.

The reducing agent used as a magnetic microparticle-separating agent isnot particularly limited. Examples of the reducing agent include sodiumborohydride, sodium hypophosphite, hydrazine, transition metal elementions (trivalent titanium ion, divalent cobalt ion, and the like),alcohols such as methanol, ethanol and 2-propanol, and ascorbic acid, aswell as ethylene glycol, glutathione, organic acids (citric acid, malicacid, tartaric acid, and the like), reducing sugars (glucose, galactose,mannose, fructose, sucrose, maltose, raffinose, stachyose, and the like)and sugar alcohols, and sorbitol. Amines may be used as the reducingagent, and such amines include, for example, aliphatic amines such aspropylamine, butylamine, hexylamine, diethylamine, dipropylamine,dimethylethylamine, diethylmethylamine, triethylamine, ethylenediamine,N,N,N′,N′-tetramethylethylenediamine, 1,3-diaminopropane,N,N,N′,N′-tetramethyl-1,3-diaminopropane, triethylenetetramine andtetraethylenepentamine; alicyclic amines such as piperidine,N-methylpiperidine, piperazine, N,N′-dimethylpiperazine, pyrrolidine,N-methylpyrrolidine, and morpholine; aromatic amines such as aniline,N-methylaniline, N,N-dimethylaniline, toluidine, anisidine, andphenetidine; and aralkylamines such as benzylamine, N-methylbenzylamine,N,N-dimethylbenzylamine, phenethylamine, xylylenediamine, andN,N,N′,N′-tetramethylxylylenediamine. Also, the above-mentioned aminesinclude alkanolamines such as methylaminoethanol, dimethylaminoethanol,triethanolamine, ethanolamine, diethanolamine, methyldiethanolamine,propanolamine, 2-(3-aminopropylamino) ethanol, butanolamine,hexanolamine, and dimethylaminopropanol.

In the reaction, a nitrogen-containing gas, a mixed gas of nitrogen andhydrogen, or an ammonia gas may be introduced into the space between theprocessing surfaces in order to nitride magnetic microparticles.Similarly, when an oxide coating is formed on magnetic microparticles, amixed gas of oxygen and an inert gas at a suitable oxygen concentrationcan be introduced into the space between the processing surfaces. Forpromoting each treatment, the space between the processing surfaces maybe heated (warmed), may be irradiated with ultraviolet ray (UV), or maybe supplied with ultrasonic energy.

When magnetic microparticles comprising a metal oxide such as magnetite(Fe₃O₄) microparticles are prepared, an aqueous solution wherein adivalent iron ion salt such as ferrous chloride, ferrous nitrate orferrous sulfate and a trivalent iron ion salt such as ferric chlorideare dissolved in a divalent/trivalent iron ion ratio of 1/2, and anaqueous solution wherein an alkaline co-precipitating agent such assodium hydroxide, potassium hydroxide or ammonia is dissolved as amagnetic microparticle-separating agent, can be used as the first andsecond fluids respectively to prepare magnetite microparticles. Theaqueous solvent is not particularly limited, and purified water such asion-exchange water and pure water can be used. For various purposes, awater-soluble organic solvent such as methanol can be mixed.

When magnetic microparticles comprising a metal sulfide are prepared, anaqueous solution wherein cobalt nitrate as a magnetic body and anothermetal (e.g. copper) nitrate are dissolved, and an aqueous solutionwherein a sulfur (S) source such as sodium sulfide (Na₂S), or a gaseoussulfur (S) source such as hydrogen sulfide (H₂S), is dissolved as amagnetic microparticle-separating agent, can be used as the first andsecond fluids respectively to prepare magnetic microparticles. Theseproducts can also be subjected to nitridization, oxidization, heatingand UV treatment, depending on the object.

A dispersant which is to be coordinated on the surfaces of magneticmicroparticles can be added to at least one of the fluids. Thedispersant is not particularly limited, and various dispersants havingexcellent dispersibility in solution and being capable of dispersingseparated magnetic microparticles excellently in solution can be used.Particularly, a polymer dispersant can be preferably used. Variouspolymer dispersants can be used. Examples of such polymer dispersantsinclude polymer dispersants having a polar group like polymerdispersants such as polyethylene imine and polyvinyl pyrrolidone,hydrocarbon polymer dispersants having in molecules a carboxylic acidgroup such as polyacrylic acid and carboxymethyl cellulose, andcopolymers like POVAL (polyvinyl alcohol) or having in one molecule apolyethylene imine moiety and a polyethylene oxide moiety. Theirmolecular weight is preferably 100,000 or less. Commercial products canalso be used. The commercial products include Solsperse 20000, Solsperse24000, Solsperse 26000, Solsperse 27000, Solsperse 28000 and Solsperse41090 (manufactured by Avecia Corporation), Disperbyk-160,Disperbyk-161, Disperbyk-162, Disperbyk-163, Disperbyk-166,Disperbyk-170, Disperbyk-180, Disperbyk-181, Disperbyk-182,Disperbyk-183, Disperbyk-184, Disperbyk-190, Disperbyk-191,Disperbyk-192, Disperbyk-2000 and Disperbyk-2001 (manufactured byBYK-Chemie), Polymer 100, Polymer 120, Polymer 150, Polymer 400, Polymer401, Polymer 402, Polymer 403, Polymer 450, Polymer 451, Polymer 452,Polymer 453, EFKA-46, EFKA-47, EFKA-48, EFKA-49, EFKA-1501, EFKA-1502,EFKA-4540 and EFKA-4550 (manufactured by EFKA Chemical Corp.), FlowlenDOPA-158, Flowlen DOPA-22, Flowlen DOPA-17, Flowlen G-700, FlowlenTG-720W, Flowlen-730W, Flowlen-740W and Flowlen-745W (manufactured byKyoeisha Chemical Co., Ltd.), Ajisper PA-111, Ajisper PB-711,AjisperPB-811, AjisperPB-821 and Ajisper PW-911 (manufactured byAjinomoto Co. Inc.), and Johncryl 678, Johncryl 679 and Johncryl 62(manufactured by Johnson Polymer B.V.). These products may be used aloneor in combination of two or more thereof. It is also possible to usehigh-molecular organic acids such as oleic acid, erucic acid, linoleicacid, polyphosphoric acids such as hexaphosphoric acid, octaphosphoricacid, tetraphosphoric acid, triphosphoric acid, acetic acid, acrylicacid, and methacrylic acid; high-molecular organic matters such aspolyvinyl pyrrolidone, polyvinyl alcohol and sodium hexamethaphosphate;thiols such as 2-mercaptoethanol, mercaptoacetic acid,2-mercaptoethylamine, β-thiodiglycol, 2,2′-thiodiacetic acid; orpolystyrene and phosphine oxides.

A pH adjusting agent for regulating pH during reaction may be added asnecessary. When the reaction conditions are made alkaline, stronglyalkaline or weakly alkaline aqueous solutions such as an aqueoussolution of sodium hydroxide, an aqueous solution of potassiumhydroxide, an aqueous solution of calcium hydroxide, an aqueous solutionof barium hydroxide, and ammonia water can be used as the pH adjustingagent.

When the reaction conditions are made acidic, strongly acidic or weaklyacidic aqueous solutions such as an aqueous solution of hydrochloricacid, an aqueous solution of nitric acid, an aqueous solution of aceticacid and an aqueous solution of citric acid as a pH adjuster can beused.

In addition, the space between the processing surfaces may be heated(warmed), may be irradiated with ultraviolet ray (UV), or may besupplied with ultrasonic energy. Particularly, when a difference intemperature is set between the first processing surface 1 and the secondprocessing surface 2, there is an advantage that since convection can begenerated in a thin film fluid, the reaction can be promoted.

Specifically for heating (warming), at least one of the processingmembers 10 and 20 can be provided for example with a heater or a jacketfor passing a heat medium, to heat (warm) the thin film fluid. Forirradiation with ultraviolet ray (UV), at least one of the processingmember 10 and the processing member 20 can be provided, for example,with an element such as UV lamp to irradiate the thin film fluid withultraviolet ray (UV) from the corresponding processing surface. Forsupplying with ultrasonic energy, at least one of the processing member10 and the processing member 20 can be provided, for example, with anultrasonic wave oscillator.

The separation is conducted in a container capable of securing adepressurized or vacuum state, and a secondary side at which the fluidafter processing is discharged can be depressurized or made vacuous toremove a gas generated during the separating reaction, to remove a gascontained in the fluid, or to remove the solvent of the fluid. Itfollows that even when separation of magnetic microparticles and removalprocessing of the solvent are simultaneously conducted, a fluidcontaining magnetic microparticles separated between the processingsurfaces is discharged in an atomized state from the processingsurfaces, and therefore, the surface area of the fluid can be increasedand the efficiency of removal of the solvent becomes extremely high.Accordingly, preparation and processing of magnetic microparticles andremoval of the solvent can be effected in substantially one step moreeasily than before.

In this manner, a magnetic fluid that is an aqueous dispersion(suspension) wherein magnetic microparticles having a volume-averageparticle size of 0.5 nm to 1000 nm, preferably 1 nm to 30 nm, morepreferably 5 nm to 11 nm, dispersed in an aqueous solvent can beprepared. When a dispersant is added to an aqueous solution having metalnitrate or the like dissolved therein, a magnetic fluid that is anaqueous dispersion (suspension) wherein magnetic microparticles havingthe dispersant coordinated thereon are dispersed can be prepared, andthe resulting magnetic microparticles are very excellent inre-dispersibility. Accordingly, a magnetic fluid in accordance with theintended use can be conveniently prepared again.

As described above, the processing apparatus can be provided with athird introduction part d3 in addition to the first introduction part d1and the second introduction part d2. In this case, a pH adjusting agent,an aqueous solution of a metal ion, a dispersant, and a magneticmicroparticle-separating agent for example can be introduced separatelythrough the respective introduction parts into the processing apparatus.By doing so, the concentration and pressure of each solution can beseparately controlled, and the reaction of forming magneticmicroparticles can be regulated more accurately. When the processingapparatus is provided with four or more introduction parts, theforegoing applies and fluids to be introduced into the processingapparatus can be subdivided in this manner.

The foregoing substantially applies where a reverse micelle method isused in the method for producing magnetic microparticles in a thin filmfluid formed between the processing surfaces arranged to be opposite toeach other so as to be able to approach to and separate from each other,at least one of which rotates relative to the other, in the presentinvention. For example, when FePt microparticles are prepared, water anda suitable dispersant such as cetyl trimethyl ammonium bromide orpentaethylene glycol dodecyl ether is added to a suitable organicsolvent such as an alkane having 7 to 12 carbon atoms, such as heptane,octane or nonane, or to an ether such as diethyl ether or dipropylether, to prepare a reverse micellar solution. An aqueous solution ofiron and platinum compounds such as iron or platinum nitrate, sulfate,hydrochloride, acetate or metal carbonyl is added to the reversemicellar solution, to prepare a reverse micellar solution containingiron and platinum compounds as a first fluid. Then, a reverse micellarsolution containing a reducing agent that is a magneticmicroparticle-separating agent is used as a second fluid to obtain FePtmicroparticle-containing suspension.

EXAMPLES

Hereinafter, the present invention is described in detail with referenceto Examples, but the present invention is not limited to Examples.

An aqueous mixed solution of iron and copper is reduced in a thin filmformed between the processing surfaces 1 and 2 arranged to be oppositeto each other so as to be able to approach to and separate from eachother, at least one of which rotates relative to the other, in use of auniformly stirring and mixing reaction apparatus shown in FIG. 1(A),thereby giving magnetic microparticles under uniform mixing in the thinfilm.

In the following Examples, the term “from the center” means “through thefirst introduction part d1” in the processing apparatus shown in FIG.1(A), the first fluid refers to the first processed fluid, and thesecond fluid refers to the second processed fluid introduced “throughthe second introduction part d2” in the processing apparatus shown inFIG. 1(A).

Example 1

While 10% hydrazine aqueous solution was sent as a first fluid from thecenter at a supply pressure/back pressure of 0.02 MPa/0.01 MPa, at arevolution number of 1000 rpm and at a sending solution temperature of80° C., an aqueous solution of 20% ferrous sulfate/18% copper sulfate/2%BYK-190 (manufactured by BYK-Chemie), just after adjusted to pH 12 withammonia water, was introduced at a rate of 10 ml/min. as a second fluidinto the space between the processing surfaces 1 and 2. An aqueousiron-copper alloy colloidal solution, that is, a magnetic fluid, wasdischarged from the processing surfaces 1 and 2.

Then, impurities were removed with a dialysis tube from the resultingaqueous iron-copper alloy colloidal solution, and iron-copper alloymicroparticles in this dispersion were observed with a transmissionelectron microscope (TEM). One hundred particles were selected at randomtherefrom, and their measured average primary particle size was 9.3 nm.The compounding ratio of iron ion/copper ion (ratio in the number ofatoms) was 10/9. The yield of the iron copper particles was 94%. Whenthe obtained iron/copper alloy microparticles were confirmed with atransmission microscope, the shape of the particles was spherical.

Example 2

While an aqueous solution of 0.3 mol/L caustic soda (sodium hydroxide)was sent as a first fluid from the center at a supply pressure/backpressure of 0.40 MPa/0.01 MPa, at a revolution number of 500 rpm and ata sending solution temperature of 95° C., a starting metal salt mixturewherein ferric chloride hexahydrate, cobalt chloride hexahydrate, nickelchloride hexahydrate, and chromium chloride hexahydrate, that is, 0.25mol/l Fe³⁺ aqueous solution, 0.10 mol/Co²⁺ aqueous solution, 0.10 mol/lNi²⁺ aqueous solution, and 0.10 mol/l Cr³⁺ aqueous solution were mixedsuch that Fe³⁺/Co²⁺/Ni²⁺/Cr³⁺ became 2/1/0.3/0.3, was introduced at arate of 10 ml/min. as a second fluid into the space between theprocessing surfaces 1 and 2. A black microparticle dispersion, that is,a magnetic fluid, was discharged from the processing surfaces.

As a result of elementary analysis of precipitates obtained by filteringa part of the obtained black microparticle dispersion, Fe was 47.6%, Co14.1%, Ni 2.9%, and Cr 2.4%. When the particle size distribution wasmeasured with a particle size distribution measuring instrumentutilizing a laser Doppler method (trade name: Microtrac UPA150,manufactured by Nikkiso Co., Ltd.), the volume-average particle size was18 nm. As a result of magnetic measurement with a physical propertymeasurement system (PPMS), saturated magnetization a of these particleswas 57.2×10⁻⁶ Wbm/kg, and holding power HcJ was 421 kA/m.

Further, the black microparticle dispersion was washed with pure waterand then vacuum-dried to give black microparticle powders. When thepowders were introduced again into ion-exchange water and stirred with ahigh-speed stirring dispersing machine (trade name: CLEARMIXmanufactured by M Technique Co., Ltd.), a black microparticle dispersionwas obtained again, its volume-average particle size was 18 nm which wasthe same as before vacuum-freeze drying, and the resulting blackmicroparticle powders were thus confirmed to be excellent inre-dispersibility.

Example 3

An alkane solution having aerosol OT, decane and 2 ml oleylamine mixedtherein was added to and mixed with a reducing agent aqueous solutionhaving NaBH₄ dissolved in water (deoxygenation: 0.1 mg/l or less), andthe resulting reverse micellar solution (0.9% NaBH₄/18.8% deoxygenatedwater/12.7% aerosol OT/65.9% decane/1.7% oleylamine) was sent as a firstfluid from the center at a supply pressure/back pressure of 0.10MPa/0.01 MPa, at a revolution number of 1000 rpm and a sending solutiontemperature of 50° C. An alkane solution having aerosol OT and decanemixed therein was added to and mixed with a metal salt aqueous solutionprepared by dissolving iron triammonium trioxalate (Fe(NH₄)₃(C₂O₄)₃) andpotassium chloroplatinate (K₂PtCl₄) in water (deoxygenated), and theresulting reverse micellar solution (1.1% (Fe (NH₄)₃(C₂O₄)₃/0.9K₂PtCl₄/18.9% deoxygenated water/12.8% aerosol OT/66.3% decane) wasintroduced as a second fluid at a rate of 10 ml/min. into the spacebetween the processing surfaces 1 and 2. A magnetic fluid, that is, areverse micellar solution containing a microparticle dispersion wasdischarged from the processing surfaces.

To destroy the resulting reverse micelle, a mixed solution ofwater/methanol (1/1) was added to the micelle to separate it intoaqueous and oil phases. The nanoparticles were dispersed in the oilphase. The oil phase was washed five times with a mixed solution ofwater/methanol (3/1).

Thereafter, the nanoparticles were sedimented by flocculation withmethanol. The supernatant was removed, and heptane was added tore-disperse the nanoparticles. Sedimentation with methanol anddispersion with heptane were repeated further three times, and heptanewas finally added to the nanoparticles to prepare a FePt (iron-platinumalloy) nanoparticle dispersion wherein the mass ratio of water to thesurfactant (water/surfactant) was 2.

Impurities were removed with a dialysis tube from the resulting FePtnanoparticle dispersion, and iron-copper alloy microparticles in thisdispersion were observed with a transmission electron microscope (TEM).One hundred particles were selected at random therefrom, and theirmeasured average primary particle size was 4.0 nm.

Comparative Example

While an aqueous solution of 0.3 mol/L caustic soda was stirred at 20000rpm at a solution temperature of 95° C. with a high-speed stirringdispersing machine (trade name: CLEARMIX manufactured by M TechniqueCo., Ltd.), a starting metal salt mixture wherein ferric chloridehexahydrate, cobalt chloride hexahydrate, nickel chloride hexahydrate,and chromium chloride hexahydrate, that is, 0.25 mol/l Fe³⁺ aqueoussolution, 0.10 mol/l Co²⁺ aqueous solution, 0.10 mol/l Ni²⁺ aqueoussolution, and 0.10 mol/l Cr²⁺ aqueous solution were mixed such thatFe³⁺/Co²⁺/Ni²⁺/Cr³⁺ became 2/1/0.3/0.3, was introduced. A blackmicroparticle dispersion, that is, a magnetic fluid, was obtained.

When the particle size distribution of the resulting blackmicroparticles was measured with a particle size distribution measuringinstrument utilizing a laser Doppler method (trade name: MicrotracUPA150, manufactured by Nikkiso Co., Ltd.), the volume-average particlesize was 970 nm.

When black microparticle powder obtained in the same manner as inExample 2 was introduced again into ion-exchange water and stirred witha high-speed stirring dispersing machine (trade name: CLEARMIXmanufactured by M Technique Co., Ltd.), a black microparticle dispersionwas obtained again, and its volume-average particle size was 1640 nmwhich was larger than before vacuum-freeze drying.

The amount of energy necessary for obtaining the magnetic microparticlesin Examples was not higher than 1/10 relative to that in ComparativeExamples, although the volume-average particle size was made smaller inExamples. From the foregoing, it was found that the production method inExamples is superior in energy efficiency.

The invention claimed is:
 1. A method for producing magneticmicroparticles, comprising: introducing at least two fluids into a spacebetween a first processing surface and a second processing surfacearranged to be opposite to each other so as to be able to approach toand separate from each other, at least one of which rotates relative tothe other, wherein at least one of the at least two fluids contains atleast one kind of a magnetic raw material, and at least another one ofthe at least two fluids contains at least one kind of a magneticmicroparticles-separating agent; generating a moving force by a fluidpressure in a direction of separating the second processing surface fromthe first processing surface; maintaining a distance between the firstprocessing surface and the second processing surface in a minute spaceby the force; forming a thin film fluid by passing the at least twofluids through the space maintained in the minute space between thefirst processing surface and the second processing surface; and themagnetic raw material reacting with the magneticmicroparticles-separating agent in the thin film fluid, whereby magneticmicroparticles are separated to obtain the magnetic microparticles. 2.The method for producing magnetic microparticles according to claim 1,wherein at least one of the at least two fluids contains a dispersant.3. The method for producing magnetic microparticles according to claim2, wherein the magnetic microparticles contain at least one kindselected from nickel, cobalt, iridium, iron, platinum, gold, silver,manganese, chromium, palladium, neodymium, samarium, gadolinium andterbium.
 4. The method for producing magnetic microparticles accordingto claim 2, wherein the magnetic microparticles contain at least onekind selected from copper, zinc, magnesium, rhenium, bismuth andsilicon.
 5. The method for producing magnetic microparticles accordingto claim 2, wherein heat or warmth is added between the processingsurfaces; ultraviolet ray (UV) is irradiated between the processingsurfaces; or ultrasonic energy is supplied between the processingsurfaces.
 6. The method for producing magnetic microparticles accordingto claim 1, wherein the magnetic microparticles contains contain atleast one kind selected from nickel, cobalt, iridium, iron, platinum,gold, silver, manganese, chromium, palladium, yttrium, neodymium,samarium, gadolinium and terbium.
 7. The method for producing magneticmicroparticles according to claim 6, wherein the magnetic microparticlescontain at least one kind selected from copper, zinc, magnesium,rhenium, bismuth and silicon.
 8. The method for producing magneticmicroparticles according to claim 1, wherein the magnetic microparticlescontain at least one kind selected from copper, zinc, magnesium,rhenium, bismuth and silicon.
 9. The method for producing magneticmicroparticles according to claim 1, wherein heat or warmth is addedbetween the processing surfaces; ultraviolet ray (UV) is irradiatedbetween the processing surfaces; or ultrasonic energy is suppliedbetween the processing surfaces.
 10. The method for producing magneticmicroparticles according to claim 1, wherein the thin film fluidcontaining the magnetic microparticles obtained by separation reactionbetween the magnetic raw material and the magneticmicroparticles-separating agent in the thin film fluid depressurizes orvacuumizes a side at which the thin film fluid is discharged from thespace between the first and second processing surfaces, thereby beingcapable of removing a solvent in the thin film fluid, or removing a gasgenerated during the separation reaction and a gas contained in the thinfilm fluid.
 11. The method for producing magnetic microparticlesaccording to claim 1, wherein the magnetic microparticles have avolume-average particle size of 0.5 nm to 1000 nm.
 12. The method forproducing magnetic microparticles according to claim 1, furthercomprising: imparting pressure to at least one of the at least twofluids by a fluid pressure imparting mechanism, rotating a firstprocessing member and a second processing member relative to each otherby a rotation drive mechanism, wherein a first processing member has thefirst processing surface and a second processing member has the secondprocessing surface, the second processing member being capable ofrelatively approaching to and separating from the first processingmember, and each of the processing surfaces constitutes part of a sealedflow path through which the at least two fluids are passed, providing atleast the second processing member with a pressure-receiving surface,wherein at least part of the pressure-receiving surface is comprised ofthe second processing surface, receiving, by the pressure-receivingsurface, pressure applied to the at least one of the at least two fluidsby the fluid pressure imparting mechanism, thereby generating the forceto move in the direction of separating the second processing surfacefrom the first processing surface, wherein the at least one of the atleast two fluids which receives pressure from the fluid pressureimparting mechanism is passed between the first and second processingsurfaces being capable of approaching to and separating from each otherand rotating relative to each other, whereby the at least one of the atleast two fluids forms a film fluid while passing between both theprocessing surfaces, introducing at least another one of the at leasttwo fluids into the space between the processing surfaces throughanother introduction path that is independent of the flow path throughwhich the at least one of the at least two fluids is passed, wherein atleast one opening leading to the another introduction path and beingarranged in at least either the first processing surface or the secondprocessing surface, and the opening is positioned downstream at a pointwhere a direction of flow of the at least one of the at least two fluidsis changed to a direction of the spiral laminar flow formed between theprocessing surfaces, and mixing the at least one of and the at leastanother one of the at least two fluids into the thin film fluid, wherebyseparation reaction occurs.
 13. The method for producing magneticmicroparticles according to claim 1, wherein the production method isconducted in a reactor capable of securing a depressurized or vacuumstate, thereby being capable of removing a solvent in the thin filmfluid, or removing a gas generated during separation reaction betweenthe magnetic raw material and the magnetic microparticles-separatingagent in the thin film fluid and a gas contained in the thin film fluidcontaining the magnetic microparticles obtained by the separationreaction.
 14. The method for producing magnetic microparticles accordingto claim 1, further comprising: forming a flat surface and a pluralityof grooves on the flat surface in the first processing surface, whereina flow path limiting part constitutes the plurality of grooves, whereinthe flow path limiting part, the first processing surface and the secondprocessing surface constitute a dynamical pressure generating mechanism,wherein a fluid pressure contains dynamic pressure proceeded from thedynamical pressure generating mechanism while at least one of the atleast two fluids is passed through the space between the firstprocessing surface and the second processing surface, and whereby thespace between the first processing surface and the second processingsurface is maintained in the minute space by the pressure of the atleast two fluids containing the dynamic pressure.
 15. A method forproducing magnetic microparticles, comprising: introducing at least twofluids into a space between a first processing surface and a secondprocessing surface arranged to be opposite to each other so as to beable to approach to and separate from each other, at least one of whichrotates relative to the other, wherein at least one of the at least twofluids is a reverse micellar solution obtained by adding a dispersantand at least one kind of aqueous magnetic raw material solution to anorganic solvent, and at least another one of the at least two fluids isa reverse micellar solution containing at least one kind of a magneticmicroparticles-separating agent; generating a moving force by a fluidpressure in a direction of separating the second processing surface fromthe first processing surface; maintaining a distance between the firstprocessing surface and the second processing surface in a minute spaceby the force; forming a thin film fluid by passing the at least twofluids through the space maintained in the minute space between thefirst processing surface and the second processing surface; and themagnetic raw material reacting with the magneticmicroparticles-separating agent in the thin film fluid, whereby magneticmicroparticles are separated to obtain the magnetic microparticles. 16.The method for producing magnetic microparticles according to claim 15,wherein the magnetic microparticles contain at least one kind selectedfrom nickel, cobalt, iridium, iron, platinum, gold, silver, manganese,chromium, palladium, yttrium, neodymium, samarium, gadolinium andterbium.
 17. The method for producing magnetic microparticles accordingto claim 15, wherein the magnetic microparticles contain at least onekind selected from copper, zinc, magnesium, rhenium, bismuth andsilicon.
 18. The method for producing magnetic microparticles accordingto claim 15, wherein heat or warmth is added between the processingsurfaces; ultraviolet ray (UV) is irradiated between the processingsurfaces; or ultrasonic energy is supplied between the processingsurfaces.
 19. The method for producing magnetic microparticles accordingto claim 15, further comprising: imparting pressure to at least one ofthe at least two fluids by a fluid pressure imparting mechanism,rotating a first processing member and a second processing memberrelative to each other by a rotation drive mechanism, wherein a firstprocessing member has the first processing surface and a secondprocessing member has the second processing surface, the secondprocessing member being capable of relatively approaching to andseparating from the first processing member, and each of the processingsurfaces constitutes part of a sealed flow path through which the atleast two fluids are passed, providing at least the second processingmember with a pressure-receiving surface, wherein at least part of thepressure-receiving surface is comprised of the second processingsurface, receiving, by the pressure-receiving surface, pressure appliedto the at least one of the at least two fluids by the fluid pressureimparting mechanism, thereby generating the force to move in thedirection of separating the second processing surface from the firstprocessing surface, wherein the at least one of the at least two fluidswhich receives pressure from the fluid pressure imparting mechanism ispassed between the first and second processing surfaces being capable ofapproaching to and separating from each other and rotating relative toeach other, whereby the at least one of the at least two fluids forms afilm fluid while passing between both the processing surfaces,introducing at least another one of the at least two fluids into thespace between the processing surfaces through another introduction paththat is independent of the flow path through which the at least one ofthe at least two fluids is passed, wherein at least one opening leadingto the another introduction path and being arranged in at least eitherthe first processing surface or the second processing surface, and theopening is positioned downstream at a point where a direction of flow ofthe at least one of the at least two fluids is changed to a direction ofthe spiral laminar flow formed between the processing surfaces, andmixing the at least one of and the at least another one of the at leasttwo fluids into the thin film fluid, whereby separation reaction occurs.20. The method for producing magnetic microparticles according to claim15, further comprising: forming a flat surface and a plurality ofgrooves on the flat surface in the first processing surface, wherein aflow path limiting part constitutes the plurality of grooves, whereinthe flow path limiting part, the first processing surface and the secondprocessing surface constitute a dynamical pressure generating mechanism,wherein a fluid pressure contains dynamic pressure proceeded from thedynamical pressure generating mechanism while at least one of the atleast two fluids is passed through the space between the firstprocessing surface and the second processing surface, and whereby thespace between the first processing surface and the second processingsurface is maintained in the minute space by the pressure of the atleast two fluids containing the dynamic pressure.